#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:46:12 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266059 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/69/7706954.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7706954
loop_
_publ_author_name
'Garg, Shipra'
'Unruh, Daniel K.'
'Krempner, Clemens'
_publ_section_title
;
 Synthesis, structures and catalytic activity of some BINOL based
 boronates and boronium salts.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5044
_journal_page_last               5049
_journal_paper_doi               10.1039/d1dt00842k
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H24 B O4, C16 H34 N4 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C58 H62 B Cl4 N4 O4 P'
_chemical_formula_weight         1062.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-18
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-02-01 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.1820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.93710(10)
_cell_length_b                   19.13750(10)
_cell_length_c                   12.85790(10)
_cell_measurement_reflns_used    54483
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      77.3430
_cell_measurement_theta_min      3.4310
_cell_volume                     2689.32(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     26.00 121.00   0.50    0.05    --   48.15  77.00 -30.00  190
  2  ω     26.00 121.00   0.50    0.05    --   48.15  77.00 -90.00  190
  3  ω     33.00 121.00   0.50    0.05    --   48.15  57.00-120.00  176
  4  ω     26.00  95.00   0.50    0.05    --   48.15  77.00  60.00  138
  5  ω     33.00 121.00   0.50    0.05    --   48.15  57.00  60.00  176
  6  ω     26.00 121.00   0.50    0.05    --   48.15  77.00 120.00  190
  7  ω     26.00 121.00   0.50    0.05    --   48.15  77.00 150.00  190
  8  ω     88.00 178.00   0.50    0.15    --  107.75 136.00  44.00  180
  9  ω     95.00 178.00   0.50    0.15    --  107.75 125.00 120.00  166
 10  ω     95.00 178.00   0.50    0.15    --  107.75 125.00 150.00  166
 11  ω     95.00 178.00   0.50    0.15    --  107.75 125.00  90.00  166
 12  ω     90.00 178.00   0.50    0.15    --  107.75 133.00-134.00  176
 13  ω     95.00 178.00   0.50    0.15    --  107.75 125.00-180.00  166
 14  ω     95.00 178.00   0.50    0.15    --  107.75  30.00  30.00  166
 15  ω     94.00 178.00   0.50    0.15    --  107.75  15.00 -30.00  168
 16  ω     94.00 178.00   0.50    0.15    --  107.75  15.00 120.00  168
 17  ω     35.00  73.00   0.50    0.15    --  107.75 -61.00 150.00   76
 18  ω     35.00 107.00   0.50    0.15    --  107.75 -77.00 150.00  144
 19  ω     35.00 107.00   0.50    0.15    --  107.75 -77.00 120.00  144
 20  ω     35.00  73.00   0.50    0.15    --  107.75 -61.00  60.00   76
 21  ω    -26.00  28.00   0.50    0.05    --   48.15 -19.00-180.00  108
 22  ω     35.00  73.00   0.50    0.15    --  107.75 -61.00-150.00   76
 23  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00-150.00  142
 24  ω     35.00 112.00   0.50    0.15    --  107.75-125.00-180.00  154
 25  ω     41.00 102.00   0.50    0.05    --   48.15-136.00 -20.00  122
 26  ω     35.00 112.00   0.50    0.15    --  107.75-125.00 -90.00  154
 27  ω     35.00 107.00   0.50    0.15    --  107.75-102.00 -45.52  144
 28  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00-180.00  142
 29  ω     41.00 120.00   0.50    0.15    --  107.75-136.00 -20.00  158
 30  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00 -30.00  142
 31  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00   0.00  142
 32  ω     35.00 106.00   0.50    0.15    --  107.75 -94.00  60.00  142
 33  ω     39.00 100.00   0.50    0.05    --   48.15-133.00 158.00  122
 34  ω     39.00 118.00   0.50    0.15    --  107.75-133.00 158.00  158
 35  ω    -94.00 -19.00   0.50    0.05    --  -48.15 136.00  44.00  150
 36  ω    -86.00 -13.00   0.50    0.15    --  -86.25 125.00 120.00  146
 37  ω    -94.00 -19.00   0.50    0.15    --  -86.25 136.00  44.00  150
 38  ω    -92.00 -17.00   0.50    0.15    --  -86.25 133.00-134.00  150
 39  ω    -92.00 -17.00   0.50    0.05    --  -48.15 133.00-134.00  150
 40  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00   0.00   70
 41  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00  30.00   70
 42  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00  90.00   70
 43  ω    -69.00 -13.00   0.50    0.15    --  -86.25  61.00 120.00  112
 44  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00  60.00   70
 45  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00 -90.00   70
 46  ω    -49.00 -14.00   0.50    0.15    --  -86.25  45.00-120.00   70
 47  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00-120.00  102
 48  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00 -90.00  102
 49  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00 -30.00  102
 50  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00  30.00  102
 51  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00  90.00  102
 52  ω    -24.00  27.00   0.50    0.05    --  -48.15  19.00 150.00  102
 53  ω   -121.00 -66.00   0.50    0.05    --  -48.15-136.00 -20.00  110
 54  ω   -159.00 -66.00   0.50    0.15    --  -86.25-136.00 -20.00  186
 55  ω   -121.00 -68.00   0.50    0.05    --  -48.15-133.00 158.00  106
 56  ω   -159.00 -68.00   0.50    0.15    --  -86.25-133.00 158.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0202987000
_diffrn_orient_matrix_UB_12      0.0784846000
_diffrn_orient_matrix_UB_13      -0.0210457000
_diffrn_orient_matrix_UB_21      0.0857223000
_diffrn_orient_matrix_UB_22      0.0179487000
_diffrn_orient_matrix_UB_23      0.0940488000
_diffrn_orient_matrix_UB_31      0.1100054000
_diffrn_orient_matrix_UB_32      0.0005394000
_diffrn_orient_matrix_UB_33      -0.0713377000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            65152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.735
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.681
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_recrystallization_method
'Slow evaporation from dichloromethane'
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 5073 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         11148
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0524P)²+1.1552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                10949
_reflns_number_total             11148
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00842k2.cif
_cod_data_source_block           R-8_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7706949--7706955.cif.'
_cod_database_code               7706954
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C118  H130  B2  N10  O12  P6  '
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.554
_shelx_estimated_absorpt_t_min   0.504
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1A-C56A = Cl2A-C56A = Cl1B-C56B = Cl2B-C56B
 1.76328 with sigma of 0.02
 Cl3A-C57A = Cl4A-C57A = Cl3B-C57B = Cl4B-C57B
 1.76328 with sigma of 0.02
 Cl3C-C57C = Cl4C-C57C
 1.76328 with sigma of 0.02
 Cl1A-Cl2A = Cl1B-Cl2B = Cl3A-Cl4A = Cl3B-Cl4B = Cl3C-Cl4C
 2.93183 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl3A \\sim Cl4A \\sim C57A \\sim Cl3B \\sim Cl4B \\sim C57B \\sim Cl3C \\sim
Cl4C \\sim C57C: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Cl1A \\sim Cl2A \\sim Cl1B \\sim Cl2B \\sim C56A \\sim C56B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 1*[Sof(Cl3A)+Sof(Cl4A)+Sof(C57A)+Sof(H57A)+Sof(H57B)]+1*[Sof(Cl3B)+Sof(Cl4B)+
 Sof(C57B)+Sof(H57C)+Sof(H57D)]+1*[Sof(Cl3C)+Sof(Cl4C)+Sof(C57C)+Sof(H57E)+
 Sof(H57F)]=1 with esd of 0
 Sof(Cl1B)=Sof(Cl2B)=Sof(C56B)=Sof(H56C)=Sof(H56D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C56A)=Sof(H56A)=Sof(H56B)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(2)
 Sof(Cl3A)=Sof(Cl4A)=Sof(C57A)=Sof(H57A)=Sof(H57B)=FVAR(3)
 Sof(Cl3B)=Sof(Cl4B)=Sof(C57B)=Sof(H57C)=Sof(H57D)=FVAR(4)
 Sof(Cl3C)=Sof(Cl4C)=Sof(C57C)=Sof(H57E)=Sof(H57F)=FVAR(5)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C56A(H56A,H56B), C56B(H56C,H56D), C57A(H57A,
 H57B), C57B(H57C,H57D), C57C(H57E,H57F)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C48(H48), C49(H49), C51(H51), C52(H52),
 C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_olex2_date_sample_data_collection 2020-09-15
_olex2_date_sample_submission    2020-09-15
_olex2_exptl_crystal_mounting_method 'MiTeGen 100 um MicroLoop'
_olex2_submission_original_sample_id kre20_31
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   6723
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.298
_oxdiff_exptl_absorpt_empirical_full_min 0.776
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.57198(15) 0.47096(9) 0.46781(13) 0.0178(3) Uani 1 1 d . . . . .
O2 O 0.47599(15) 0.38666(9) 0.34644(13) 0.0168(3) Uani 1 1 d . . . . .
O3 O 0.54216(15) 0.34649(9) 0.50599(13) 0.0175(3) Uani 1 1 d . . . . .
O4 O 0.37861(16) 0.43393(9) 0.50056(13) 0.0174(3) Uani 1 1 d . . . . .
C17 C 0.6624(2) 0.48234(12) 0.40126(19) 0.0164(5) Uani 1 1 d . . . . .
C18 C 0.6388(2) 0.49395(12) 0.29616(18) 0.0153(4) Uani 1 1 d . . . . .
C019 C 0.4596(2) 0.54812(13) 0.19014(18) 0.0162(5) Uani 1 1 d . . . . .
C19 C 0.7401(2) 0.50198(12) 0.22935(19) 0.0158(4) Uani 1 1 d . . . . .
C20 C 0.7253(2) 0.50350(13) 0.11891(19) 0.0176(5) Uani 1 1 d . . . . .
H20 H 0.647280 0.499122 0.088161 0.021 Uiso 1 1 calc R U . . .
C21 C 0.8235(2) 0.51126(15) 0.0571(2) 0.0225(5) Uani 1 1 d . . . . .
H21 H 0.811516 0.511727 -0.014938 0.027 Uiso 1 1 calc R U . . .
C22 C 0.9431(2) 0.51859(15) 0.1017(2) 0.0245(5) Uani 1 1 d . . . . .
H22 H 1.009143 0.525542 0.059444 0.029 Uiso 1 1 calc R U . . .
C23 C 0.9607(2) 0.51538(14) 0.2075(2) 0.0221(5) Uani 1 1 d . . . . .
H23 H 1.039479 0.519378 0.236604 0.027 Uiso 1 1 calc R U . . .
C24 C 0.8614(2) 0.50609(13) 0.2734(2) 0.0181(5) Uani 1 1 d . . . . .
C25 C 0.8797(2) 0.49924(14) 0.3831(2) 0.0204(5) Uani 1 1 d . . . . .
H25 H 0.958091 0.503669 0.413029 0.024 Uiso 1 1 calc R U . . .
C26 C 0.7839(2) 0.48628(13) 0.44486(19) 0.0191(5) Uani 1 1 d . . . . .
H26 H 0.797820 0.479946 0.516031 0.023 Uiso 1 1 calc R U . . .
C27 C 0.5105(2) 0.49272(13) 0.25363(18) 0.0156(5) Uani 1 1 d . . . . .
C28 C 0.4362(2) 0.43689(13) 0.27778(17) 0.0154(5) Uani 1 1 d . . . . .
C29 C 0.3182(2) 0.42889(13) 0.22977(18) 0.0177(5) Uani 1 1 d . . . . .
H29 H 0.271721 0.389600 0.244037 0.021 Uiso 1 1 calc R U . . .
C30 C 0.2725(2) 0.47851(14) 0.16274(19) 0.0183(5) Uani 1 1 d . . . . .
H30 H 0.197027 0.471507 0.128612 0.022 Uiso 1 1 calc R U . . .
C31 C 0.3391(2) 0.54070(13) 0.14458(18) 0.0168(5) Uani 1 1 d . . . . .
C32 C 0.2873(2) 0.59734(14) 0.08611(19) 0.0195(5) Uani 1 1 d . . . . .
H32 H 0.209302 0.592574 0.055542 0.023 Uiso 1 1 calc R U . . .
C33 C 0.3495(2) 0.65844(15) 0.07391(19) 0.0213(5) Uani 1 1 d . . . . .
H33 H 0.313357 0.695166 0.036681 0.026 Uiso 1 1 calc R U . . .
C34 C 0.4687(2) 0.66559(14) 0.11800(18) 0.0197(5) Uani 1 1 d . . . . .
H34 H 0.511600 0.706973 0.108927 0.024 Uiso 1 1 calc R U . . .
C35 C 0.5222(2) 0.61197(13) 0.17428(19) 0.0180(5) Uani 1 1 d . . . . .
H35 H 0.601043 0.617627 0.202602 0.022 Uiso 1 1 calc R U . . .
C36 C 0.5510(2) 0.34677(13) 0.61204(18) 0.0163(5) Uani 1 1 d . . . . .
C37 C 0.4481(2) 0.34530(12) 0.67103(18) 0.0156(4) Uani 1 1 d . . . . .
C38 C 0.4645(2) 0.35071(12) 0.78237(19) 0.0163(5) Uani 1 1 d . . . . .
C39 C 0.3655(2) 0.36245(14) 0.8491(2) 0.0201(5) Uani 1 1 d . . . . .
H39 H 0.286268 0.364837 0.820403 0.024 Uiso 1 1 calc R U . . .
C40 C 0.3839(3) 0.37028(15) 0.9541(2) 0.0245(5) Uani 1 1 d . . . . .
H40 H 0.317378 0.378195 0.995492 0.029 Uiso 1 1 calc R U . . .
C41 C 0.5027(3) 0.36649(16) 1.0002(2) 0.0269(6) Uani 1 1 d . . . . .
H41 H 0.514369 0.370905 1.071958 0.032 Uiso 1 1 calc R U . . .
C42 C 0.6005(2) 0.35630(15) 0.9391(2) 0.0233(5) Uani 1 1 d . . . . .
H42 H 0.678766 0.353974 0.969772 0.028 Uiso 1 1 calc R U . . .
C43 C 0.5848(2) 0.34919(13) 0.82949(19) 0.0186(5) Uani 1 1 d . . . . .
C44 C 0.6864(2) 0.34458(14) 0.7651(2) 0.0209(5) Uani 1 1 d . . . . .
H44 H 0.764886 0.341161 0.795114 0.025 Uiso 1 1 calc R U . . .
C45 C 0.6704(2) 0.34509(13) 0.6593(2) 0.0188(5) Uani 1 1 d . . . . .
H45 H 0.738272 0.344331 0.617881 0.023 Uiso 1 1 calc R U . . .
C46 C 0.3240(2) 0.34377(13) 0.61930(18) 0.0159(5) Uani 1 1 d . . . . .
C47 C 0.2958(2) 0.38996(13) 0.53870(19) 0.0166(5) Uani 1 1 d . . . . .
C48 C 0.1737(2) 0.39734(13) 0.49891(19) 0.0186(5) Uani 1 1 d . . . . .
H48 H 0.156051 0.429678 0.446466 0.022 Uiso 1 1 calc R U . . .
C49 C 0.0814(2) 0.35745(14) 0.5367(2) 0.0214(5) Uani 1 1 d . . . . .
H49 H 0.001012 0.365160 0.513393 0.026 Uiso 1 1 calc R U . . .
C50 C 0.1076(2) 0.30474(14) 0.6109(2) 0.0194(5) Uani 1 1 d . . . . .
C51 C 0.0150(2) 0.25888(15) 0.6453(2) 0.0263(6) Uani 1 1 d . . . . .
H51 H -0.065469 0.265539 0.621444 0.032 Uiso 1 1 calc R U . . .
C52 C 0.0419(3) 0.20524(15) 0.7125(2) 0.0283(6) Uani 1 1 d . . . . .
H52 H -0.019742 0.175857 0.734388 0.034 Uiso 1 1 calc R U . . .
C53 C 0.1640(3) 0.19484(14) 0.7484(2) 0.0241(5) Uani 1 1 d . . . . .
H53 H 0.183032 0.157583 0.792587 0.029 Uiso 1 1 calc R U . . .
C54 C 0.2548(2) 0.23898(13) 0.7190(2) 0.0194(5) Uani 1 1 d . . . . .
H54 H 0.334506 0.231415 0.744406 0.023 Uiso 1 1 calc R U . . .
C55 C 0.2305(2) 0.29626(13) 0.65049(19) 0.0176(5) Uani 1 1 d . . . . .
B1 B 0.4926(2) 0.40934(15) 0.4557(2) 0.0166(5) Uani 1 1 d . . . . .
P1 P 0.44582(5) 0.66610(3) 0.63997(4) 0.01582(13) Uani 1 1 d . . . . .
N1 N 0.3888(2) 0.73747(11) 0.68860(17) 0.0186(4) Uani 1 1 d . . . . .
H1 H 0.427(3) 0.7720(19) 0.667(3) 0.022 Uiso 1 1 d . U . . .
N2 N 0.3899(2) 0.63338(11) 0.53178(16) 0.0187(4) Uani 1 1 d . . . . .
N3 N 0.4253(2) 0.60379(11) 0.72519(16) 0.0196(4) Uani 1 1 d . . . . .
N4 N 0.5859(2) 0.68900(12) 0.61636(17) 0.0207(4) Uani 1 1 d . . . . .
C1 C 0.2603(2) 0.75629(14) 0.7143(2) 0.0197(5) Uani 1 1 d . . . . .
C2 C 0.2718(3) 0.81636(16) 0.7915(3) 0.0310(6) Uani 1 1 d . . . . .
H2A H 0.312327 0.800284 0.854599 0.046 Uiso 1 1 calc R U . . .
H2B H 0.191705 0.833258 0.806597 0.046 Uiso 1 1 calc R U . . .
H2C H 0.318459 0.853438 0.762174 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1916(3) 0.69630(15) 0.7643(2) 0.0244(5) Uani 1 1 d . . . . .
H3A H 0.191963 0.656265 0.719290 0.037 Uiso 1 1 calc R U . . .
H3B H 0.108756 0.710262 0.774939 0.037 Uiso 1 1 calc R U . . .
H3C H 0.231050 0.684674 0.829980 0.037 Uiso 1 1 calc R U . . .
C4 C 0.1911(3) 0.78015(17) 0.6152(2) 0.0309(6) Uani 1 1 d . . . . .
H4A H 0.234463 0.818021 0.584406 0.046 Uiso 1 1 calc R U . . .
H4B H 0.110671 0.795504 0.632072 0.046 Uiso 1 1 calc R U . . .
H4C H 0.184653 0.741940 0.566978 0.046 Uiso 1 1 calc R U . . .
C5 C 0.4126(2) 0.66450(16) 0.42843(18) 0.0238(5) Uani 1 1 d . . . . .
H5A H 0.476523 0.639369 0.393880 0.029 Uiso 1 1 calc R U . . .
H5B H 0.435886 0.713247 0.435075 0.029 Uiso 1 1 calc R U . . .
C6 C 0.2908(3) 0.65694(15) 0.36944(19) 0.0246(5) Uani 1 1 d . . . . .
H6A H 0.301233 0.655498 0.294899 0.030 Uiso 1 1 calc R U . . .
H6B H 0.235791 0.694886 0.385459 0.030 Uiso 1 1 calc R U . . .
C7 C 0.2438(3) 0.58737(15) 0.4094(2) 0.0246(5) Uani 1 1 d . . . . .
H7A H 0.283545 0.548458 0.376173 0.029 Uiso 1 1 calc R U . . .
H7B H 0.155976 0.583364 0.397272 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2773(2) 0.58967(14) 0.5259(2) 0.0204(5) Uani 1 1 d . . . . .
H8A H 0.212378 0.610866 0.564471 0.025 Uiso 1 1 calc R U . . .
H8B H 0.293371 0.543144 0.553088 0.025 Uiso 1 1 calc R U . . .
C9 C 0.4442(3) 0.61534(16) 0.8390(2) 0.0268(6) Uani 1 1 d . . . . .
H9A H 0.371653 0.602194 0.875422 0.032 Uiso 1 1 calc R U . . .
H9B H 0.462172 0.664102 0.853421 0.032 Uiso 1 1 calc R U . . .
C10 C 0.5531(3) 0.56902(19) 0.8734(3) 0.0406(8) Uani 1 1 d . . . . .
H10A H 0.619323 0.597224 0.903231 0.049 Uiso 1 1 calc R U . . .
H10B H 0.528819 0.535244 0.924955 0.049 Uiso 1 1 calc R U . . .
C11 C 0.5929(3) 0.53238(16) 0.7760(2) 0.0309(6) Uani 1 1 d . . . . .
H11A H 0.618031 0.484720 0.790984 0.037 Uiso 1 1 calc R U . . .
H11B H 0.659861 0.557057 0.745024 0.037 Uiso 1 1 calc R U . . .
C12 C 0.4783(3) 0.53402(14) 0.7046(2) 0.0238(5) Uani 1 1 d . . . . .
H12A H 0.498819 0.529350 0.632238 0.029 Uiso 1 1 calc R U . . .
H12B H 0.421975 0.497023 0.722055 0.029 Uiso 1 1 calc R U . . .
C13 C 0.6646(3) 0.65216(17) 0.5420(2) 0.0317(6) Uani 1 1 d . . . . .
H13A H 0.659446 0.674093 0.473933 0.038 Uiso 1 1 calc R U . . .
H13B H 0.641358 0.603428 0.534937 0.038 Uiso 1 1 calc R U . . .
C14 C 0.7924(3) 0.6592(2) 0.5912(3) 0.0393(7) Uani 1 1 d . . . . .
H14A H 0.810586 0.620922 0.638707 0.047 Uiso 1 1 calc R U . . .
H14B H 0.853528 0.660346 0.538546 0.047 Uiso 1 1 calc R U . . .
C15 C 0.7882(3) 0.72771(18) 0.6487(3) 0.0357(7) Uani 1 1 d . . . . .
H15A H 0.797332 0.766778 0.601551 0.043 Uiso 1 1 calc R U . . .
H15B H 0.852134 0.730042 0.702958 0.043 Uiso 1 1 calc R U . . .
C16 C 0.6622(3) 0.72795(16) 0.6949(3) 0.0300(6) Uani 1 1 d . . . . .
H16A H 0.663637 0.704514 0.761796 0.036 Uiso 1 1 calc R U . . .
H16B H 0.632272 0.775248 0.703250 0.036 Uiso 1 1 calc R U . . .
Cl1A Cl 1.00339(11) 0.52775(7) 0.67178(11) 0.0416(4) Uani 0.627(2) 1 d D U P A
1
Cl2A Cl 1.0683(2) 0.45152(14) 0.86192(13) 0.0830(8) Uani 0.627(2) 1 d D U P A 1
C56A C 1.1216(7) 0.4829(5) 0.7449(7) 0.0428(16) Uani 0.627(2) 1 d D U P A 1
H56A H 1.151182 0.444190 0.704187 0.051 Uiso 0.627(2) 1 calc R U P A 1
H56B H 1.189498 0.514546 0.759060 0.051 Uiso 0.627(2) 1 calc R U P A 1
Cl1B Cl 1.1503(2) 0.51143(13) 0.85644(17) 0.0404(6) Uani 0.373(2) 1 d D U P A 2
Cl2B Cl 0.9252(2) 0.4723(2) 0.7409(2) 0.0667(9) Uani 0.373(2) 1 d D U P A 2
C56B C 1.0855(13) 0.4876(11) 0.7343(14) 0.053(3) Uani 0.373(2) 1 d D U P A 2
H56C H 1.125068 0.445581 0.710110 0.063 Uiso 0.373(2) 1 calc R U P A 2
H56D H 1.099533 0.524545 0.684517 0.063 Uiso 0.373(2) 1 calc R U P A 2
Cl3A Cl -0.0527(2) 0.83090(10) 0.92204(18) 0.0559(5) Uani 0.649(4) 1 d D U P B
1
Cl4A Cl -0.0774(4) 0.68284(15) 0.9557(3) 0.1202(15) Uani 0.649(4) 1 d D U P B 1
C57A C -0.1039(12) 0.7667(6) 1.0065(10) 0.091(2) Uani 0.649(4) 1 d D U P B 1
H57A H -0.190731 0.772837 1.016347 0.110 Uiso 0.649(4) 1 calc R U P B 1
H57B H -0.061387 0.771385 1.073711 0.110 Uiso 0.649(4) 1 calc R U P B 1
Cl3B Cl -0.0154(8) 0.8429(4) 0.9744(8) 0.102(2) Uani 0.280(4) 1 d D U P C 2
Cl4B Cl -0.1329(10) 0.6978(5) 0.9512(7) 0.115(2) Uani 0.280(4) 1 d D U P C 2
C57B C -0.068(3) 0.7674(13) 1.029(2) 0.091(3) Uani 0.280(4) 1 d D U P C 2
H57C H -0.129004 0.780903 1.077706 0.110 Uiso 0.280(4) 1 calc R U P C 2
H57D H 0.000057 0.747563 1.069655 0.110 Uiso 0.280(4) 1 calc R U P C 2
Cl3C Cl 0.063(2) 0.7340(12) 1.0428(16) 0.095(4) Uani 0.072(2) 1 d D U P D 3
Cl4C Cl -0.127(2) 0.7845(14) 0.9020(19) 0.103(3) Uani 0.072(2) 1 d D U P D 3
C57C C -0.028(6) 0.807(3) 1.010(5) 0.091(3) Uani 0.072(2) 1 d D U P D 3
H57E H 0.023654 0.846350 0.991834 0.109 Uiso 0.072(2) 1 calc R U P D 3
H57F H -0.075614 0.820880 1.068738 0.109 Uiso 0.072(2) 1 calc R U P D 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -1 0 0.1418
1 5 8 0.1296
7 4 0 0.1339
6 1 -4 0.1223
2 -3 -8 0.1215
-1 -5 -7 0.1302
-1 -10 5 0.1263
-6 0 5 0.1533
-4 10 1 0.1607
-1 12 -2 0.1310
3 8 -5 0.1388
6 0 -5 0.1272
6 -6 -3 0.1193
4 -11 0 0.1149
-1 -11 4 0.1215
5 9 -1 0.1425
1 12 3 0.1328
-5 -9 1 0.1298
-1 -12 -3 0.1198
4 -5 -6 0.1188
2 -10 -5 0.1229
1 12 -1 0.1288
0 12 0 0.1365
3 -11 -2 0.1171
0 -12 0 0.1216
7 -4 0 0.1218
0 -5 8 0.1297
-6 5 -3 0.1531
-2 6 -7 0.1413
1 4 -8 0.1204
-7 -1 0 0.1403
-2 -2 -8 0.1348
1 -1 -8 0.1203
0 1 8 0.1224
6 2 3 0.1438
-6 3 -3 0.1447
-2 3 -8 0.1344
0 -3 8 0.1204
7 -2 0 0.1204
-5 -8 -1 0.1372
0 -9 -6 0.1196
-6 -6 0 0.1364
0 11 3 0.1361
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 O1 B1 120.43(19) . . ?
C28 O2 B1 115.69(18) . . ?
C36 O3 B1 116.79(19) . . ?
C47 O4 B1 122.44(19) . . ?
O1 C17 C18 122.1(2) . . ?
O1 C17 C26 117.0(2) . . ?
C18 C17 C26 120.8(2) . . ?
C17 C18 C19 118.8(2) . . ?
C17 C18 C27 119.7(2) . . ?
C19 C18 C27 121.4(2) . . ?
C31 C019 C27 119.4(2) . . ?
C35 C019 C27 122.5(2) . . ?
C35 C019 C31 118.0(2) . . ?
C20 C19 C18 122.6(2) . . ?
C20 C19 C24 117.7(2) . . ?
C24 C19 C18 119.8(2) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.3(2) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.6(2) . . ?
C22 C21 H21 119.7 . . ?
C21 C22 H22 120.3 . . ?
C23 C22 C21 119.4(2) . . ?
C23 C22 H22 120.3 . . ?
C22 C23 H23 119.3 . . ?
C22 C23 C24 121.3(2) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 C19 119.6(2) . . ?
C23 C24 C25 121.6(2) . . ?
C25 C24 C19 118.8(2) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 C24 120.8(2) . . ?
C26 C25 H25 119.6 . . ?
C17 C26 H26 119.7 . . ?
C25 C26 C17 120.5(2) . . ?
C25 C26 H26 119.7 . . ?
C019 C27 C18 122.5(2) . . ?
C28 C27 C18 118.9(2) . . ?
C28 C27 C019 118.5(2) . . ?
O2 C28 C27 120.8(2) . . ?
O2 C28 C29 117.9(2) . . ?
C27 C28 C29 121.2(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(2) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 119.7 . . ?
C29 C30 C31 120.6(2) . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C019 119.1(2) . . ?
C30 C31 C32 121.9(2) . . ?
C32 C31 C019 118.9(2) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.5(2) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 120.2 . . ?
C32 C33 C34 119.7(2) . . ?
C34 C33 H33 120.2 . . ?
C33 C34 H34 119.7 . . ?
C35 C34 C33 120.6(2) . . ?
C35 C34 H34 119.7 . . ?
C019 C35 H35 119.3 . . ?
C34 C35 C019 121.4(2) . . ?
C34 C35 H35 119.3 . . ?
O3 C36 C37 121.4(2) . . ?
O3 C36 C45 117.2(2) . . ?
C37 C36 C45 121.3(2) . . ?
C36 C37 C38 118.2(2) . . ?
C36 C37 C46 120.2(2) . . ?
C38 C37 C46 121.5(2) . . ?
C39 C38 C37 122.8(2) . . ?
C39 C38 C43 117.2(2) . . ?
C43 C38 C37 119.9(2) . . ?
C38 C39 H39 119.1 . . ?
C40 C39 C38 121.8(2) . . ?
C40 C39 H39 119.1 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.6(2) . . ?
C41 C40 H40 119.7 . . ?
C40 C41 H41 120.2 . . ?
C42 C41 C40 119.6(2) . . ?
C42 C41 H41 120.2 . . ?
C41 C42 H42 119.4 . . ?
C41 C42 C43 121.2(2) . . ?
C43 C42 H42 119.4 . . ?
C42 C43 C38 119.6(2) . . ?
C44 C43 C38 119.0(2) . . ?
C44 C43 C42 121.3(2) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 C43 120.6(2) . . ?
C45 C44 H44 119.7 . . ?
C36 C45 H45 119.8 . . ?
C44 C45 C36 120.5(2) . . ?
C44 C45 H45 119.8 . . ?
C47 C46 C37 119.6(2) . . ?
C47 C46 C55 118.1(2) . . ?
C55 C46 C37 122.3(2) . . ?
O4 C47 C46 122.5(2) . . ?
O4 C47 C48 116.4(2) . . ?
C46 C47 C48 120.8(2) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 C47 120.8(2) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 H49 119.8 . . ?
C48 C49 C50 120.4(2) . . ?
C50 C49 H49 119.8 . . ?
C49 C50 C51 121.5(2) . . ?
C49 C50 C55 119.1(2) . . ?
C51 C50 C55 119.4(2) . . ?
C50 C51 H51 119.3 . . ?
C52 C51 C50 121.4(3) . . ?
C52 C51 H51 119.3 . . ?
C51 C52 H52 120.3 . . ?
C51 C52 C53 119.4(2) . . ?
C53 C52 H52 120.3 . . ?
C52 C53 H53 119.6 . . ?
C54 C53 C52 120.7(2) . . ?
C54 C53 H53 119.6 . . ?
C53 C54 H54 119.2 . . ?
C53 C54 C55 121.7(2) . . ?
C55 C54 H54 119.2 . . ?
C50 C55 C46 119.9(2) . . ?
C54 C55 C46 122.7(2) . . ?
C54 C55 C50 117.3(2) . . ?
O1 B1 O2 112.8(2) . . ?
O1 B1 O4 101.99(19) . . ?
O3 B1 O1 114.0(2) . . ?
O3 B1 O2 102.11(19) . . ?
O3 B1 O4 113.3(2) . . ?
O4 B1 O2 113.1(2) . . ?
N1 P1 N3 106.73(11) . . ?
N2 P1 N1 120.86(11) . . ?
N2 P1 N3 103.61(11) . . ?
N2 P1 N4 105.65(11) . . ?
N4 P1 N1 102.76(12) . . ?
N4 P1 N3 118.19(12) . . ?
P1 N1 H1 110(2) . . ?
C1 N1 P1 131.20(18) . . ?
C1 N1 H1 111(2) . . ?
C5 N2 P1 122.78(18) . . ?
C5 N2 C8 110.3(2) . . ?
C8 N2 P1 122.95(16) . . ?
C9 N3 P1 122.13(18) . . ?
C12 N3 P1 118.10(17) . . ?
C12 N3 C9 105.6(2) . . ?
C13 N4 P1 124.19(19) . . ?
C16 N4 P1 120.99(19) . . ?
C16 N4 C13 110.5(2) . . ?
N1 C1 C2 105.7(2) . . ?
N1 C1 C3 113.1(2) . . ?
N1 C1 C4 109.1(2) . . ?
C2 C1 C3 108.8(2) . . ?
C2 C1 C4 110.2(2) . . ?
C4 C1 C3 109.9(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 111.0 . . ?
N2 C5 H5B 111.0 . . ?
N2 C5 C6 103.6(2) . . ?
H5A C5 H5B 109.0 . . ?
C6 C5 H5A 111.0 . . ?
C6 C5 H5B 111.0 . . ?
C5 C6 H6A 111.3 . . ?
C5 C6 H6B 111.3 . . ?
C5 C6 C7 102.5(2) . . ?
H6A C6 H6B 109.2 . . ?
C7 C6 H6A 111.3 . . ?
C7 C6 H6B 111.3 . . ?
C6 C7 H7A 111.1 . . ?
C6 C7 H7B 111.1 . . ?
C6 C7 C8 103.5(2) . . ?
H7A C7 H7B 109.0 . . ?
C8 C7 H7A 111.1 . . ?
C8 C7 H7B 111.1 . . ?
N2 C8 C7 103.5(2) . . ?
N2 C8 H8A 111.1 . . ?
N2 C8 H8B 111.1 . . ?
C7 C8 H8A 111.1 . . ?
C7 C8 H8B 111.1 . . ?
H8A C8 H8B 109.0 . . ?
N3 C9 H9A 110.5 . . ?
N3 C9 H9B 110.5 . . ?
N3 C9 C10 106.0(2) . . ?
H9A C9 H9B 108.7 . . ?
C10 C9 H9A 110.5 . . ?
C10 C9 H9B 110.5 . . ?
C9 C10 H10A 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
C11 C10 C9 105.8(2) . . ?
C11 C10 H10A 110.6 . . ?
C11 C10 H10B 110.6 . . ?
C10 C11 H11A 111.1 . . ?
C10 C11 H11B 111.1 . . ?
C10 C11 C12 103.5(2) . . ?
H11A C11 H11B 109.0 . . ?
C12 C11 H11A 111.1 . . ?
C12 C11 H11B 111.1 . . ?
N3 C12 C11 103.2(2) . . ?
N3 C12 H12A 111.1 . . ?
N3 C12 H12B 111.1 . . ?
C11 C12 H12A 111.1 . . ?
C11 C12 H12B 111.1 . . ?
H12A C12 H12B 109.1 . . ?
N4 C13 H13A 111.0 . . ?
N4 C13 H13B 111.0 . . ?
N4 C13 C14 103.6(2) . . ?
H13A C13 H13B 109.0 . . ?
C14 C13 H13A 111.0 . . ?
C14 C13 H13B 111.0 . . ?
C13 C14 H14A 111.0 . . ?
C13 C14 H14B 111.0 . . ?
H14A C14 H14B 109.0 . . ?
C15 C14 C13 103.7(3) . . ?
C15 C14 H14A 111.0 . . ?
C15 C14 H14B 111.0 . . ?
C14 C15 H15A 111.0 . . ?
C14 C15 H15B 111.0 . . ?
C14 C15 C16 103.8(2) . . ?
H15A C15 H15B 109.0 . . ?
C16 C15 H15A 111.0 . . ?
C16 C15 H15B 111.0 . . ?
N4 C16 C15 103.1(2) . . ?
N4 C16 H16A 111.1 . . ?
N4 C16 H16B 111.1 . . ?
C15 C16 H16A 111.1 . . ?
C15 C16 H16B 111.1 . . ?
H16A C16 H16B 109.1 . . ?
Cl1A C56A H56A 109.4 . . ?
Cl1A C56A H56B 109.4 . . ?
Cl2A C56A Cl1A 111.2(4) . . ?
Cl2A C56A H56A 109.4 . . ?
Cl2A C56A H56B 109.4 . . ?
H56A C56A H56B 108.0 . . ?
Cl1B C56B Cl2B 111.4(9) . . ?
Cl1B C56B H56C 109.4 . . ?
Cl1B C56B H56D 109.4 . . ?
Cl2B C56B H56C 109.4 . . ?
Cl2B C56B H56D 109.4 . . ?
H56C C56B H56D 108.0 . . ?
Cl3A C57A Cl4A 110.5(7) . . ?
Cl3A C57A H57A 109.6 . . ?
Cl3A C57A H57B 109.6 . . ?
Cl4A C57A H57A 109.6 . . ?
Cl4A C57A H57B 109.6 . . ?
H57A C57A H57B 108.1 . . ?
Cl3B C57B Cl4B 122.0(16) . . ?
Cl3B C57B H57C 106.8 . . ?
Cl3B C57B H57D 106.8 . . ?
Cl4B C57B H57C 106.8 . . ?
Cl4B C57B H57D 106.8 . . ?
H57C C57B H57D 106.7 . . ?
Cl3C C57C Cl4C 108(2) . . ?
Cl3C C57C H57E 110.1 . . ?
Cl3C C57C H57F 110.1 . . ?
Cl4C C57C H57E 110.1 . . ?
Cl4C C57C H57F 110.1 . . ?
H57E C57C H57F 108.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C17 1.350(3) . ?
O1 B1 1.469(3) . ?
O2 C28 1.365(3) . ?
O2 B1 1.475(3) . ?
O3 C36 1.363(3) . ?
O3 B1 1.460(3) . ?
O4 C47 1.343(3) . ?
O4 B1 1.471(3) . ?
C17 C18 1.384(3) . ?
C17 C26 1.424(3) . ?
C18 C19 1.436(3) . ?
C18 C27 1.486(3) . ?
C019 C27 1.438(3) . ?
C019 C31 1.428(3) . ?
C019 C35 1.419(3) . ?
C19 C20 1.423(3) . ?
C19 C24 1.425(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.369(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.415(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.368(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.414(4) . ?
C24 C25 1.424(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.361(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.385(3) . ?
C28 C29 1.417(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.364(4) . ?
C30 H30 0.9300 . ?
C30 C31 1.419(4) . ?
C31 C32 1.425(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.365(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.408(3) . ?
C34 H34 0.9300 . ?
C34 C35 1.373(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.380(3) . ?
C36 C45 1.420(3) . ?
C37 C38 1.440(3) . ?
C37 C46 1.489(3) . ?
C38 C39 1.424(3) . ?
C38 C43 1.428(3) . ?
C39 H39 0.9300 . ?
C39 C40 1.365(4) . ?
C40 H40 0.9300 . ?
C40 C41 1.410(4) . ?
C41 H41 0.9300 . ?
C41 C42 1.366(4) . ?
C42 H42 0.9300 . ?
C42 C43 1.420(3) . ?
C43 C44 1.414(4) . ?
C44 H44 0.9300 . ?
C44 C45 1.365(4) . ?
C45 H45 0.9300 . ?
C46 C47 1.388(3) . ?
C46 C55 1.437(3) . ?
C47 C48 1.419(3) . ?
C48 H48 0.9300 . ?
C48 C49 1.369(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.410(4) . ?
C50 C51 1.423(4) . ?
C50 C55 1.428(3) . ?
C51 H51 0.9300 . ?
C51 C52 1.367(4) . ?
C52 H52 0.9300 . ?
C52 C53 1.411(4) . ?
C53 H53 0.9300 . ?
C53 C54 1.368(4) . ?
C54 H54 0.9300 . ?
C54 C55 1.425(4) . ?
P1 N1 1.635(2) . ?
P1 N2 1.624(2) . ?
P1 N3 1.641(2) . ?
P1 N4 1.633(2) . ?
N1 H1 0.83(4) . ?
N1 C1 1.500(3) . ?
N2 C5 1.486(3) . ?
N2 C8 1.488(3) . ?
N3 C9 1.487(3) . ?
N3 C12 1.483(3) . ?
N4 C13 1.489(4) . ?
N4 C16 1.485(4) . ?
C1 C2 1.522(4) . ?
C1 C3 1.527(4) . ?
C1 C4 1.526(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.515(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.524(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.529(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.537(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.514(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.525(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.518(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.506(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.521(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
Cl1A C56A 1.789(6) . ?
Cl2A C56A 1.741(10) . ?
C56A H56A 0.9700 . ?
C56A H56B 0.9700 . ?
Cl1B C56B 1.759(16) . ?
Cl2B C56B 1.783(15) . ?
C56B H56C 0.9700 . ?
C56B H56D 0.9700 . ?
Cl3A C57A 1.746(10) . ?
Cl4A C57A 1.761(12) . ?
C57A H57A 0.9700 . ?
C57A H57B 0.9700 . ?
Cl3B C57B 1.71(2) . ?
Cl4B C57B 1.80(2) . ?
C57B H57C 0.9700 . ?
C57B H57D 0.9700 . ?
Cl3C C57C 1.76(3) . ?
Cl4C C57C 1.78(3) . ?
C57C H57E 0.9700 . ?
C57C H57F 0.9700 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C17 C18 C19 -176.7(2) . . . . ?
O1 C17 C18 C27 -1.1(3) . . . . ?
O1 C17 C26 C25 -178.5(2) . . . . ?
O2 C28 C29 C30 178.2(2) . . . . ?
O3 C36 C37 C38 -175.7(2) . . . . ?
O3 C36 C37 C46 -0.4(4) . . . . ?
O3 C36 C45 C44 -179.4(2) . . . . ?
O4 C47 C48 C49 -176.6(2) . . . . ?
C17 O1 B1 O2 -30.3(3) . . . . ?
C17 O1 B1 O3 85.6(3) . . . . ?
C17 O1 B1 O4 -151.9(2) . . . . ?
C17 C18 C19 C20 170.3(2) . . . . ?
C17 C18 C19 C24 -7.3(3) . . . . ?
C17 C18 C27 C019 128.9(2) . . . . ?
C17 C18 C27 C28 -49.6(3) . . . . ?
C18 C17 C26 C25 -2.2(4) . . . . ?
C18 C19 C20 C21 180.0(2) . . . . ?
C18 C19 C24 C23 -178.8(2) . . . . ?
C18 C19 C24 C25 2.5(4) . . . . ?
C18 C27 C28 O2 5.5(3) . . . . ?
C18 C27 C28 C29 -172.5(2) . . . . ?
C019 C27 C28 O2 -173.1(2) . . . . ?
C019 C27 C28 C29 8.9(3) . . . . ?
C019 C31 C32 C33 -0.8(4) . . . . ?
C19 C18 C27 C019 -55.6(3) . . . . ?
C19 C18 C27 C28 125.9(2) . . . . ?
C19 C20 C21 C22 -0.5(4) . . . . ?
C19 C24 C25 C26 2.5(4) . . . . ?
C20 C19 C24 C23 3.5(4) . . . . ?
C20 C19 C24 C25 -175.2(2) . . . . ?
C20 C21 C22 C23 2.3(4) . . . . ?
C21 C22 C23 C24 -1.1(4) . . . . ?
C22 C23 C24 C19 -1.8(4) . . . . ?
C22 C23 C24 C25 176.8(3) . . . . ?
C23 C24 C25 C26 -176.2(3) . . . . ?
C24 C19 C20 C21 -2.4(4) . . . . ?
C24 C25 C26 C17 -2.8(4) . . . . ?
C26 C17 C18 C19 7.2(3) . . . . ?
C26 C17 C18 C27 -177.2(2) . . . . ?
C27 C18 C19 C20 -5.2(4) . . . . ?
C27 C18 C19 C24 177.2(2) . . . . ?
C27 C019 C31 C30 -0.2(3) . . . . ?
C27 C019 C31 C32 176.9(2) . . . . ?
C27 C019 C35 C34 -176.4(2) . . . . ?
C27 C28 C29 C30 -3.8(3) . . . . ?
C28 O2 B1 O1 -53.6(3) . . . . ?
C28 O2 B1 O3 -176.42(18) . . . . ?
C28 O2 B1 O4 61.5(3) . . . . ?
C28 C29 C30 C31 -3.6(4) . . . . ?
C29 C30 C31 C019 5.5(3) . . . . ?
C29 C30 C31 C32 -171.6(2) . . . . ?
C30 C31 C32 C33 176.3(2) . . . . ?
C31 C019 C27 C18 174.6(2) . . . . ?
C31 C019 C27 C28 -6.8(3) . . . . ?
C31 C019 C35 C34 0.8(3) . . . . ?
C31 C32 C33 C34 1.4(4) . . . . ?
C32 C33 C34 C35 -0.9(4) . . . . ?
C33 C34 C35 C019 -0.2(4) . . . . ?
C35 C019 C27 C18 -8.3(4) . . . . ?
C35 C019 C27 C28 170.3(2) . . . . ?
C35 C019 C31 C30 -177.5(2) . . . . ?
C35 C019 C31 C32 -0.3(3) . . . . ?
C36 O3 B1 O1 67.5(3) . . . . ?
C36 O3 B1 O2 -170.44(19) . . . . ?
C36 O3 B1 O4 -48.5(3) . . . . ?
C36 C37 C38 C39 168.3(2) . . . . ?
C36 C37 C38 C43 -7.3(3) . . . . ?
C36 C37 C46 C47 -47.4(3) . . . . ?
C36 C37 C46 C55 133.3(3) . . . . ?
C37 C36 C45 C44 -2.5(4) . . . . ?
C37 C38 C39 C40 -177.2(3) . . . . ?
C37 C38 C43 C42 178.4(2) . . . . ?
C37 C38 C43 C44 2.0(4) . . . . ?
C37 C46 C47 O4 4.0(3) . . . . ?
C37 C46 C47 C48 -170.1(2) . . . . ?
C37 C46 C55 C50 169.3(2) . . . . ?
C37 C46 C55 C54 -11.9(4) . . . . ?
C38 C37 C46 C47 127.8(3) . . . . ?
C38 C37 C46 C55 -51.5(3) . . . . ?
C38 C39 C40 C41 -0.4(4) . . . . ?
C38 C43 C44 C45 3.3(4) . . . . ?
C39 C38 C43 C42 2.6(3) . . . . ?
C39 C38 C43 C44 -173.8(2) . . . . ?
C39 C40 C41 C42 1.3(4) . . . . ?
C40 C41 C42 C43 -0.2(4) . . . . ?
C41 C42 C43 C38 -1.8(4) . . . . ?
C41 C42 C43 C44 174.6(3) . . . . ?
C42 C43 C44 C45 -173.1(2) . . . . ?
C43 C38 C39 C40 -1.5(4) . . . . ?
C43 C44 C45 C36 -3.1(4) . . . . ?
C45 C36 C37 C38 7.6(4) . . . . ?
C45 C36 C37 C46 -177.1(2) . . . . ?
C46 C37 C38 C39 -6.9(4) . . . . ?
C46 C37 C38 C43 177.5(2) . . . . ?
C46 C47 C48 C49 -2.1(4) . . . . ?
C47 O4 B1 O1 -156.47(19) . . . . ?
C47 O4 B1 O2 82.1(3) . . . . ?
C47 O4 B1 O3 -33.5(3) . . . . ?
C47 C46 C55 C50 -10.0(3) . . . . ?
C47 C46 C55 C54 168.8(2) . . . . ?
C47 C48 C49 C50 -4.5(4) . . . . ?
C48 C49 C50 C51 -174.9(3) . . . . ?
C48 C49 C50 C55 3.6(4) . . . . ?
C49 C50 C51 C52 176.1(3) . . . . ?
C49 C50 C55 C46 3.7(4) . . . . ?
C49 C50 C55 C54 -175.2(2) . . . . ?
C50 C51 C52 C53 -0.2(5) . . . . ?
C51 C50 C55 C46 -177.8(2) . . . . ?
C51 C50 C55 C54 3.4(4) . . . . ?
C51 C52 C53 C54 1.9(4) . . . . ?
C52 C53 C54 C55 -0.8(4) . . . . ?
C53 C54 C55 C46 179.4(2) . . . . ?
C53 C54 C55 C50 -1.8(4) . . . . ?
C55 C46 C47 O4 -176.6(2) . . . . ?
C55 C46 C47 C48 9.3(3) . . . . ?
C55 C50 C51 C52 -2.4(4) . . . . ?
B1 O1 C17 C18 63.0(3) . . . . ?
B1 O1 C17 C26 -120.8(2) . . . . ?
B1 O2 C28 C27 68.1(3) . . . . ?
B1 O2 C28 C29 -113.8(2) . . . . ?
B1 O3 C36 C37 69.2(3) . . . . ?
B1 O3 C36 C45 -113.9(2) . . . . ?
B1 O4 C47 C46 58.9(3) . . . . ?
B1 O4 C47 C48 -126.7(2) . . . . ?
P1 N1 C1 C2 159.7(2) . . . . ?
P1 N1 C1 C3 40.7(3) . . . . ?
P1 N1 C1 C4 -81.9(3) . . . . ?
P1 N2 C5 C6 -140.85(19) . . . . ?
P1 N2 C8 C7 166.11(18) . . . . ?
P1 N3 C9 C10 -114.8(3) . . . . ?
P1 N3 C12 C11 102.0(2) . . . . ?
P1 N4 C13 C14 -146.4(2) . . . . ?
P1 N4 C16 C15 171.3(2) . . . . ?
N1 P1 N2 C5 74.6(2) . . . . ?
N1 P1 N2 C8 -80.7(2) . . . . ?
N1 P1 N3 C9 -40.9(2) . . . . ?
N1 P1 N3 C12 -174.94(19) . . . . ?
N1 P1 N4 C13 -159.4(2) . . . . ?
N1 P1 N4 C16 46.0(2) . . . . ?
N2 P1 N1 C1 53.7(3) . . . . ?
N2 P1 N3 C9 -169.5(2) . . . . ?
N2 P1 N3 C12 56.5(2) . . . . ?
N2 P1 N4 C13 -31.9(3) . . . . ?
N2 P1 N4 C16 173.6(2) . . . . ?
N2 C5 C6 C7 -35.4(3) . . . . ?
N3 P1 N1 C1 -64.1(3) . . . . ?
N3 P1 N2 C5 -166.1(2) . . . . ?
N3 P1 N2 C8 38.7(2) . . . . ?
N3 P1 N4 C13 83.4(2) . . . . ?
N3 P1 N4 C16 -71.1(2) . . . . ?
N3 C9 C10 C11 0.1(4) . . . . ?
N4 P1 N1 C1 170.9(2) . . . . ?
N4 P1 N2 C5 -41.1(2) . . . . ?
N4 P1 N2 C8 163.59(19) . . . . ?
N4 P1 N3 C9 74.1(2) . . . . ?
N4 P1 N3 C12 -59.9(2) . . . . ?
N4 C13 C14 C15 -30.6(3) . . . . ?
C5 N2 C8 C7 8.1(3) . . . . ?
C5 C6 C7 C8 40.9(3) . . . . ?
C6 C7 C8 N2 -30.1(3) . . . . ?
C8 N2 C5 C6 17.2(3) . . . . ?
C9 N3 C12 C11 -38.8(3) . . . . ?
C9 C10 C11 C12 -23.3(3) . . . . ?
C10 C11 C12 N3 38.2(3) . . . . ?
C12 N3 C9 C10 24.0(3) . . . . ?
C13 N4 C16 C15 13.6(3) . . . . ?
C13 C14 C15 C16 39.6(3) . . . . ?
C14 C15 C16 N4 -32.5(3) . . . . ?
C16 N4 C13 C14 10.5(3) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9981 -0.9999 -0.0035 -0.0378 -0.1896 -0.2201
0.7562 4.8777 7.5851 0.2078 0.8657 -0.4553
6.7724 3.7045 -0.0187 0.1537 0.6453 0.7483
6.1081 0.7041 -4.4989 0.0260 0.1131 0.9932
2.3643 -3.2147 -7.6684 -0.1389 -0.5762 0.8054
-1.4076 -5.1023 -7.3594 -0.2170 -0.9044 0.3674
-0.6738 -10.1299 4.7885 -0.8821 0.2108 -0.4212
-5.6938 -0.1837 5.2359 -0.0090 0.0010 -1.0000
-4.1419 10.0682 0.6485 0.8606 -0.1133 -0.4965
-1.3110 11.6415 -2.4074 0.9910 -0.1298 0.0338
2.9770 8.2884 -5.2637 0.7009 -0.0911 0.7075
5.6976 0.1871 -5.2299 0.0091 -0.0001 1.0000
5.6508 -6.0459 -3.2613 -0.5206 0.0692 0.8510
3.5754 -10.7283 0.0697 -0.9160 0.1205 0.3826
-0.7547 -10.8205 4.0288 -0.9187 0.1200 -0.3763
4.6888 9.1953 -1.2443 0.6527 0.4500 0.6095
1.3908 11.5388 2.5559 0.8236 0.5667 -0.0231
-4.5693 -9.4174 1.0611 -0.6687 -0.4609 -0.5834
-1.2019 -11.5215 -2.7233 -0.8225 -0.5659 0.0558
4.3516 -5.2950 -5.7455 -0.3830 -0.2624 0.8857
1.9041 -9.5609 -4.9187 -0.6855 -0.4710 0.5552
1.0705 12.1133 -1.3904 0.9582 0.1784 0.2235
-0.1847 12.4100 -0.2563 0.9831 0.1828 0.0047
2.7886 -11.0137 -2.1651 -0.8754 -0.1623 0.4553
0.1750 -12.4100 0.2651 -0.9831 -0.1828 -0.0064
6.7588 -3.7907 -0.0248 -0.4342 0.5090 0.7432
0.0780 -4.8986 7.6591 -0.5472 0.6391 -0.5404
-5.8719 5.1501 -2.9079 0.5846 -0.6844 -0.4357
-1.9038 5.5335 -7.0386 0.6211 -0.7258 0.2957
1.0960 4.3042 -7.7646 0.4790 -0.5590 0.6768
-7.0298 -1.2804 -0.4853 0.0524 -0.6712 -0.7394
-2.0984 -1.6757 -7.7941 0.0751 -0.9430 0.3243
0.9431 -1.2371 -8.2665 0.0577 -0.7188 0.6928
0.2821 1.4456 8.2643 -0.0662 0.8274 -0.5577
6.2961 1.6502 3.4119 -0.0701 0.8902 0.4501
-6.2486 2.9338 -3.1593 0.4236 -0.7801 -0.4604
-1.7984 3.1673 -7.7022 0.4472 -0.8217 0.3533
-0.0117 -2.7764 8.1290 -0.3887 0.7137 -0.5827
6.9625 -2.2021 0.4004 -0.3226 0.5950 0.7362
-5.0407 -8.4730 -1.2276 -0.5368 -0.6996 -0.4715
0.1528 -8.5233 -6.0719 -0.5443 -0.7109 0.4454
-6.2873 -5.7186 -0.2250 -0.3165 -0.6628 -0.6787
0.2857 11.2663 3.4833 0.8051 0.5543 -0.2110
