#------------------------------------------------------------------------------
#$Date: 2022-05-03 02:20:48 +0300 (Tue, 03 May 2022) $
#$Revision: 274817 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/01/7710156.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_7710156
loop_
_publ_author_name
'Merschel, Arne'
'Vishnevskiy, Yury V.'
'Neumann, Beate'
'Stammler, Georg'
'Ghadwal, Rajendra S.'
_publ_section_title
;
 Crystalline phosphino-functionalized mesoionic olefins (p-MIOs)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01314B
_journal_year                    2022
_chemical_formula_moiety         'C52 H55 N2 P'
_chemical_formula_sum            'C52 H55 N2 P'
_chemical_formula_weight         738.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-31
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-11-12 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                75.720(6)
_cell_angle_beta                 87.335(5)
_cell_angle_gamma                70.184(6)
_cell_formula_units_Z            2
_cell_length_a                   10.5080(7)
_cell_length_b                   10.6031(6)
_cell_length_c                   20.8200(14)
_cell_measurement_reflns_used    4467
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.6220
_cell_measurement_theta_min      4.3560
_cell_volume                     2113.2(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -29.00   1.00   17.50    --  -38.50 -38.00  30.00   76
  2  ω   -110.00 -18.00   1.00   17.50    --  -38.50 -38.00 -60.00   92
  3  ω    -72.00  -6.00   1.00   17.50    --  -38.50 125.00  90.00   66
  4  ω     34.00  61.00   1.00   17.50    --   43.07 -99.00  90.00   27
  5  ω     20.00 110.00   1.00   17.50    --   43.07  57.00-120.00   90
  6  ω     59.00  96.00   1.00   17.50    --   43.07-125.00 -90.00   37
  7  ω     45.00 103.00   1.00   40.00    --  106.24 -94.00  90.00   58
  8  ω     27.00 107.00   1.00   40.00    --  106.24 -94.00 -30.00   80
  9  ω     34.00 107.00   1.00   40.00    --  106.24 -30.00   0.00   73
 10  ω     26.00 104.00   1.00   40.00    --  106.24 -94.00 150.00   78
 11  ω     49.00 125.00   1.00   40.00    --  106.24 -30.00 -90.00   76
 12  ω     43.00 130.00   1.00   40.00    --  106.24 -61.00-180.00   87
 13  ω    103.00 130.00   1.00   40.00    --  106.24 125.00 150.00   27
 14  ω    138.00 175.00   1.00   40.00    --  106.24 125.00 150.00   37
 15  ω     48.00 127.00   1.00   40.00    --  106.24 -30.00  90.00   79
 16  ω     99.00 125.00   1.00   40.00    --  106.24 125.00 120.00   26
 17  ω     66.00 178.00   1.00   40.00    --  106.24  15.00 -60.00  112
 18  ω     78.00 107.00   1.00   40.00    --  106.24-100.00-109.38   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0884797000
_diffrn_orient_matrix_UB_12      0.0179865000
_diffrn_orient_matrix_UB_13      -0.0603549000
_diffrn_orient_matrix_UB_21      0.0788143000
_diffrn_orient_matrix_UB_22      0.0610659000
_diffrn_orient_matrix_UB_23      0.0371404000
_diffrn_orient_matrix_UB_31      0.1013999000
_diffrn_orient_matrix_UB_32      -0.1460498000
_diffrn_orient_matrix_UB_33      0.0285801000
_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  0.0385
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15647
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.479
_diffrn_reflns_theta_min         4.386
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.889
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0427P)²+0.5720P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6141
_reflns_number_total             8322
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01314b2.cif
_cod_data_source_block           compound_4b
_cod_database_code               7710156
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C52H55N2P
_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.
;
_diffrn_oxdiff_digest_frames
;
0119e3adcf5eff393f1d88b78aa3cd8cba01150628f
;
_diffrn_oxdiff_digest_hkl
;
01a811c5c0d722b2d98e0aecf434070dd98bfb
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C23(H23), C26(H26), C35(H35), C38(H38)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C31(H31), C32(H32),
  C33(H33), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C)
;
_olex2_date_sample_data_collection 2020-07-30
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.867
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
P1 P 0.91930(5) 0.63042(5) 0.38314(2) 0.01962(11) Uani 1 1 d . . . . .
N1 N 0.71329(15) 0.77249(15) 0.28931(8) 0.0170(3) Uani 1 1 d . . . . .
N2 N 0.79058(15) 0.74436(15) 0.19329(7) 0.0171(3) Uani 1 1 d . . . . .
C1 C 0.67483(18) 0.79079(18) 0.22672(9) 0.0165(4) Uani 1 1 d . . . . .
C2 C 0.85418(18) 0.71132(18) 0.29964(9) 0.0187(4) Uani 1 1 d . . . . .
C3 C 0.90842(18) 0.69971(18) 0.23598(9) 0.0180(4) Uani 1 1 d . . . . .
C4 C 1.04387(19) 0.65179(19) 0.22362(10) 0.0211(4) Uani 1 1 d . . . . .
H4 H 1.097332 0.639066 0.260619 0.025 Uiso 1 1 calc R . . . .
C5 C 1.12674(19) 0.61541(19) 0.16833(10) 0.0212(4) Uani 1 1 d . . . . .
C6 C 1.10130(19) 0.6823(2) 0.10067(10) 0.0229(4) Uani 1 1 d . . . . .
H6 H 1.022865 0.758135 0.087350 0.028 Uiso 1 1 calc R . . . .
C7 C 1.1910(2) 0.6374(2) 0.05319(11) 0.0283(4) Uani 1 1 d . . . . .
H7 H 1.170420 0.682701 0.008681 0.034 Uiso 1 1 calc R . . . .
C8 C 1.3102(2) 0.5266(2) 0.07082(11) 0.0328(5) Uani 1 1 d . . . . .
H8 H 1.369044 0.496511 0.038686 0.039 Uiso 1 1 calc R . . . .
C9 C 1.3399(2) 0.4615(2) 0.13764(12) 0.0344(5) Uani 1 1 d . . . . .
H9 H 1.420591 0.388389 0.150626 0.041 Uiso 1 1 calc R . . . .
C10 C 1.2501(2) 0.5046(2) 0.18499(11) 0.0268(4) Uani 1 1 d . . . . .
H10 H 1.271925 0.458943 0.229387 0.032 Uiso 1 1 calc R . . . .
C11 C 0.53358(19) 0.83968(19) 0.20084(9) 0.0208(4) Uani 1 1 d . . . . .
C12 C 0.4337(2) 0.9460(2) 0.22157(10) 0.0252(4) Uani 1 1 d . . . . .
H12 H 0.457524 0.991566 0.249369 0.030 Uiso 1 1 calc R . . . .
C13 C 0.2993(2) 0.9840(2) 0.20102(11) 0.0327(5) Uani 1 1 d . . . . .
H13 H 0.234130 1.056465 0.214254 0.039 Uiso 1 1 calc R . . . .
C14 C 0.2615(2) 0.9153(3) 0.16106(11) 0.0337(5) Uani 1 1 d . . . . .
H14 H 0.170822 0.938431 0.148943 0.040 Uiso 1 1 calc R . . . .
C15 C 0.3597(2) 0.8118(2) 0.13928(11) 0.0302(5) Uani 1 1 d . . . . .
H15 H 0.334872 0.766481 0.111665 0.036 Uiso 1 1 calc R . . . .
C16 C 0.4948(2) 0.7749(2) 0.15815(10) 0.0245(4) Uani 1 1 d . . . . .
H16 H 0.560038 0.706575 0.142283 0.029 Uiso 1 1 calc R . . . .
C17 C 0.62519(18) 0.80284(18) 0.34279(9) 0.0179(4) Uani 1 1 d . . . . .
C18 C 0.61971(19) 0.91794(19) 0.36604(9) 0.0206(4) Uani 1 1 d . . . . .
C19 C 0.5391(2) 0.9405(2) 0.41955(10) 0.0260(4) Uani 1 1 d . . . . .
H19 H 0.532899 1.015282 0.436756 0.031 Uiso 1 1 calc R . . . .
C20 C 0.4675(2) 0.8538(2) 0.44789(10) 0.0288(4) Uani 1 1 d . . . . .
H20 H 0.414043 0.871263 0.483704 0.035 Uiso 1 1 calc R . . . .
C21 C 0.4748(2) 0.7419(2) 0.42358(10) 0.0268(4) Uani 1 1 d . . . . .
H21 H 0.424664 0.685800 0.442607 0.032 Uiso 1 1 calc R . . . .
C22 C 0.55614(19) 0.7121(2) 0.37093(9) 0.0215(4) Uani 1 1 d . . . . .
C23 C 0.6960(2) 1.0157(2) 0.33493(10) 0.0247(4) Uani 1 1 d . . . . .
H23 H 0.770478 0.965997 0.310659 0.030 Uiso 1 1 calc R . . . .
C24 C 0.7575(2) 1.0599(2) 0.38676(12) 0.0327(5) Uani 1 1 d . . . . .
H24A H 0.686781 1.122191 0.406128 0.049 Uiso 1 1 calc GR . . . .
H24B H 0.819084 1.105584 0.366081 0.049 Uiso 1 1 calc GR . . . .
H24C H 0.805473 0.979892 0.420740 0.049 Uiso 1 1 calc GR . . . .
C25 C 0.6068(3) 1.1449(2) 0.28528(12) 0.0389(5) Uani 1 1 d . . . . .
H25A H 0.581388 1.118786 0.248116 0.058 Uiso 1 1 calc GR . . . .
H25B H 0.656095 1.207425 0.270188 0.058 Uiso 1 1 calc GR . . . .
H25C H 0.526843 1.189580 0.306402 0.058 Uiso 1 1 calc GR . . . .
C26 C 0.5690(2) 0.5840(2) 0.34758(10) 0.0261(4) Uani 1 1 d . . . . .
H26 H 0.630250 0.580537 0.310604 0.031 Uiso 1 1 calc R . . . .
C27 C 0.4336(2) 0.5873(2) 0.32261(12) 0.0340(5) Uani 1 1 d . . . . .
H27A H 0.372641 0.587406 0.358428 0.051 Uiso 1 1 calc GR . . . .
H27B H 0.446945 0.507301 0.305875 0.051 Uiso 1 1 calc GR . . . .
H27C H 0.395790 0.669387 0.287781 0.051 Uiso 1 1 calc GR . . . .
C28 C 0.6322(3) 0.4535(2) 0.40336(13) 0.0398(6) Uani 1 1 d . . . . .
H28A H 0.714541 0.455990 0.420246 0.060 Uiso 1 1 calc GR . . . .
H28B H 0.651580 0.373036 0.386249 0.060 Uiso 1 1 calc GR . . . .
H28C H 0.569930 0.449913 0.438444 0.060 Uiso 1 1 calc GR . . . .
C29 C 0.78769(18) 0.7519(2) 0.12362(9) 0.0194(4) Uani 1 1 d . . . . .
C30 C 0.82399(19) 0.6287(2) 0.10283(10) 0.0227(4) Uani 1 1 d . . . . .
C31 C 0.8147(2) 0.6407(2) 0.03476(11) 0.0288(4) Uani 1 1 d . . . . .
H31 H 0.838085 0.561290 0.019046 0.035 Uiso 1 1 calc R . . . .
C32 C 0.7715(2) 0.7687(2) -0.00950(10) 0.0326(5) Uani 1 1 d . . . . .
H32 H 0.764331 0.774405 -0.054565 0.039 Uiso 1 1 calc R . . . .
C33 C 0.7386(2) 0.8886(2) 0.01222(10) 0.0296(5) Uani 1 1 d . . . . .
H33 H 0.710800 0.973921 -0.018447 0.036 Uiso 1 1 calc R . . . .
C34 C 0.74650(18) 0.8830(2) 0.07953(9) 0.0214(4) Uani 1 1 d . . . . .
C35 C 0.8723(2) 0.4871(2) 0.15160(11) 0.0296(5) Uani 1 1 d . . . . .
H35 H 0.907474 0.498615 0.191774 0.036 Uiso 1 1 calc R . . . .
C36 C 0.7576(3) 0.4302(3) 0.17175(18) 0.0603(9) Uani 1 1 d . . . . .
H36A H 0.693689 0.487938 0.195965 0.090 Uiso 1 1 calc GR . . . .
H36B H 0.793558 0.337918 0.199236 0.090 Uiso 1 1 calc GR . . . .
H36C H 0.713186 0.429004 0.132765 0.090 Uiso 1 1 calc GR . . . .
C37 C 0.9872(2) 0.3817(2) 0.12543(12) 0.0320(5) Uani 1 1 d . . . . .
H37A H 0.954169 0.362510 0.087966 0.048 Uiso 1 1 calc GR . . . .
H37B H 1.020893 0.297812 0.159681 0.048 Uiso 1 1 calc GR . . . .
H37C H 1.058966 0.418328 0.112173 0.048 Uiso 1 1 calc GR . . . .
C38 C 0.7206(2) 1.0143(2) 0.10321(10) 0.0265(4) Uani 1 1 d . . . . .
H38 H 0.685283 0.998080 0.147775 0.032 Uiso 1 1 calc R . . . .
C39 C 0.6154(3) 1.1416(2) 0.06050(13) 0.0413(6) Uani 1 1 d . . . . .
H39A H 0.649767 1.165291 0.017320 0.062 Uiso 1 1 calc GR . . . .
H39B H 0.596409 1.217522 0.080937 0.062 Uiso 1 1 calc GR . . . .
H39C H 0.533771 1.122117 0.056325 0.062 Uiso 1 1 calc GR . . . .
C40 C 0.8529(3) 1.0402(3) 0.10968(16) 0.0476(7) Uani 1 1 d . . . . .
H40A H 0.914109 0.962465 0.140460 0.071 Uiso 1 1 calc GR . . . .
H40B H 0.835246 1.121955 0.125517 0.071 Uiso 1 1 calc GR . . . .
H40C H 0.892711 1.052368 0.067153 0.071 Uiso 1 1 calc GR . . . .
C41 C 1.01840(19) 0.73049(19) 0.40152(10) 0.0218(4) Uani 1 1 d . . . . .
C42 C 1.0279(2) 0.7332(2) 0.46776(10) 0.0282(4) Uani 1 1 d . . . . .
H42 H 0.995444 0.675596 0.500358 0.034 Uiso 1 1 calc R . . . .
C43 C 1.0850(2) 0.8202(2) 0.48573(11) 0.0308(5) Uani 1 1 d . . . . .
H43 H 1.090677 0.820997 0.530067 0.037 Uiso 1 1 calc R . . . .
C44 C 1.1334(2) 0.9058(2) 0.43769(12) 0.0315(5) Uani 1 1 d . . . . .
H44 H 1.169320 0.966435 0.449350 0.038 Uiso 1 1 calc R . . . .
C45 C 1.1285(2) 0.9011(2) 0.37174(11) 0.0297(5) Uani 1 1 d . . . . .
H45 H 1.164055 0.956484 0.339591 0.036 Uiso 1 1 calc R . . . .
C46 C 1.0709(2) 0.8145(2) 0.35343(10) 0.0251(4) Uani 1 1 d . . . . .
H46 H 1.067265 0.812513 0.309153 0.030 Uiso 1 1 calc R . . . .
C47 C 1.04714(19) 0.46979(19) 0.37284(10) 0.0222(4) Uani 1 1 d . . . . .
C48 C 1.0082(2) 0.3894(2) 0.33907(11) 0.0270(4) Uani 1 1 d . . . . .
H48 H 0.920711 0.420628 0.320706 0.032 Uiso 1 1 calc R . . . .
C49 C 1.0985(2) 0.2635(2) 0.33262(12) 0.0336(5) Uani 1 1 d . . . . .
H49 H 1.071787 0.211407 0.309449 0.040 Uiso 1 1 calc R . . . .
C50 C 1.2283(2) 0.2149(2) 0.36053(13) 0.0354(5) Uani 1 1 d . . . . .
H50 H 1.289310 0.130926 0.355746 0.042 Uiso 1 1 calc R . . . .
C51 C 1.2668(2) 0.2921(2) 0.39564(12) 0.0331(5) Uani 1 1 d . . . . .
H51 H 1.353199 0.258617 0.415435 0.040 Uiso 1 1 calc R . . . .
C52 C 1.1770(2) 0.4197(2) 0.40157(11) 0.0271(4) Uani 1 1 d . . . . .
H52 H 1.204129 0.471400 0.424790 0.032 Uiso 1 1 calc R . . . .
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'
N N 0.0311 0.0180 '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
-1 0 -1 0.0046
1 0 1 0.0070
-4 -1 10 0.0295
4 1 -10 0.0295
-3 5 -2 0.0409
3 -5 2 0.0309
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
C2 P1 C41 105.63(9) . . ?
C2 P1 C47 101.24(9) . . ?
C41 P1 C47 104.03(9) . . ?
C1 N1 C2 111.80(15) . . ?
C1 N1 C17 126.25(15) . . ?
C2 N1 C17 121.87(15) . . ?
C1 N2 C3 110.92(15) . . ?
C1 N2 C29 122.27(15) . . ?
C3 N2 C29 126.65(15) . . ?
N1 C1 N2 106.90(15) . . ?
N1 C1 C11 125.56(16) . . ?
N2 C1 C11 127.32(16) . . ?
N1 C2 P1 117.65(13) . . ?
N1 C2 C3 106.49(15) . . ?
C3 C2 P1 133.60(14) . . ?
N2 C3 C2 103.59(15) . . ?
C4 C3 N2 131.20(17) . . ?
C4 C3 C2 125.18(17) . . ?
C3 C4 H4 111.3 . . ?
C3 C4 C5 137.43(18) . . ?
C5 C4 H4 111.3 . . ?
C6 C5 C4 127.56(18) . . ?
C6 C5 C10 116.07(18) . . ?
C10 C5 C4 116.28(18) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 C5 121.35(19) . . ?
C7 C6 H6 119.3 . . ?
C6 C7 H7 119.3 . . ?
C8 C7 C6 121.3(2) . . ?
C8 C7 H7 119.3 . . ?
C7 C8 H8 120.8 . . ?
C7 C8 C9 118.45(19) . . ?
C9 C8 H8 120.8 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(2) . . ?
C10 C9 H9 119.8 . . ?
C5 C10 H10 118.8 . . ?
C9 C10 C5 122.3(2) . . ?
C9 C10 H10 118.8 . . ?
C12 C11 C1 120.92(17) . . ?
C16 C11 C1 120.66(17) . . ?
C16 C11 C12 118.30(18) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.6(2) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.6(2) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.3(2) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.7(2) . . ?
C16 C15 H15 119.7 . . ?
C11 C16 H16 119.8 . . ?
C15 C16 C11 120.48(19) . . ?
C15 C16 H16 119.8 . . ?
C18 C17 N1 117.87(16) . . ?
C22 C17 N1 118.36(16) . . ?
C22 C17 C18 123.67(17) . . ?
C17 C18 C23 123.05(17) . . ?
C19 C18 C17 116.44(18) . . ?
C19 C18 C23 120.51(17) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 C18 121.32(19) . . ?
C20 C19 H19 119.3 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.72(19) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.70(19) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 C26 123.03(17) . . ?
C21 C22 C17 117.12(18) . . ?
C21 C22 C26 119.84(18) . . ?
C18 C23 H23 107.6 . . ?
C18 C23 C24 112.32(17) . . ?
C18 C23 C25 112.35(17) . . ?
C24 C23 H23 107.6 . . ?
C24 C23 C25 109.04(17) . . ?
C25 C23 H23 107.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26 107.9 . . ?
C22 C26 C27 112.11(17) . . ?
C22 C26 C28 110.22(18) . . ?
C27 C26 H26 107.9 . . ?
C27 C26 C28 110.70(18) . . ?
C28 C26 H26 107.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N2 118.82(17) . . ?
C34 C29 N2 118.06(16) . . ?
C34 C29 C30 123.11(18) . . ?
C29 C30 C35 122.16(18) . . ?
C31 C30 C29 117.01(19) . . ?
C31 C30 C35 120.83(18) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 C30 120.95(19) . . ?
C32 C31 H31 119.5 . . ?
C31 C32 H32 119.6 . . ?
C31 C32 C33 120.9(2) . . ?
C33 C32 H32 119.6 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.8(2) . . ?
C34 C33 H33 119.6 . . ?
C29 C34 C38 121.74(17) . . ?
C33 C34 C29 117.27(18) . . ?
C33 C34 C38 120.86(18) . . ?
C30 C35 H35 107.3 . . ?
C30 C35 C37 112.70(17) . . ?
C36 C35 C30 112.2(2) . . ?
C36 C35 H35 107.3 . . ?
C36 C35 C37 109.65(18) . . ?
C37 C35 H35 107.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38 107.1 . . ?
C34 C38 C39 113.88(18) . . ?
C39 C38 H38 107.1 . . ?
C40 C38 C34 110.41(17) . . ?
C40 C38 H38 107.1 . . ?
C40 C38 C39 111.00(19) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 P1 116.55(15) . . ?
C46 C41 P1 124.19(15) . . ?
C46 C41 C42 118.87(19) . . ?
C41 C42 H42 119.5 . . ?
C43 C42 C41 121.0(2) . . ?
C43 C42 H42 119.5 . . ?
C42 C43 H43 120.1 . . ?
C44 C43 C42 119.8(2) . . ?
C44 C43 H43 120.1 . . ?
C43 C44 H44 120.1 . . ?
C43 C44 C45 119.8(2) . . ?
C45 C44 H44 120.1 . . ?
C44 C45 H45 119.7 . . ?
C46 C45 C44 120.6(2) . . ?
C46 C45 H45 119.7 . . ?
C41 C46 H46 120.1 . . ?
C45 C46 C41 119.85(19) . . ?
C45 C46 H46 120.1 . . ?
C48 C47 P1 118.06(15) . . ?
C52 C47 P1 122.87(16) . . ?
C52 C47 C48 118.87(18) . . ?
C47 C48 H48 119.7 . . ?
C49 C48 C47 120.7(2) . . ?
C49 C48 H48 119.7 . . ?
C48 C49 H49 119.9 . . ?
C50 C49 C48 120.2(2) . . ?
C50 C49 H49 119.9 . . ?
C49 C50 H50 120.2 . . ?
C49 C50 C51 119.6(2) . . ?
C51 C50 H50 120.2 . . ?
C50 C51 H51 119.7 . . ?
C50 C51 C52 120.5(2) . . ?
C52 C51 H51 119.7 . . ?
C47 C52 C51 120.1(2) . . ?
C47 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
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
P1 C2 1.7898(19) . ?
P1 C41 1.829(2) . ?
P1 C47 1.8312(19) . ?
N1 C1 1.330(2) . ?
N1 C2 1.403(2) . ?
N1 C17 1.442(2) . ?
N2 C1 1.375(2) . ?
N2 C3 1.430(2) . ?
N2 C29 1.434(2) . ?
C1 C11 1.476(3) . ?
C2 C3 1.435(3) . ?
C3 C4 1.375(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.460(3) . ?
C5 C6 1.404(3) . ?
C5 C10 1.411(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.390(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.384(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.389(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.384(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.398(3) . ?
C11 C16 1.397(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.387(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.381(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.381(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.387(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.403(3) . ?
C17 C22 1.397(3) . ?
C18 C19 1.387(3) . ?
C18 C23 1.524(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.384(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.379(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.391(3) . ?
C22 C26 1.515(3) . ?
C23 H23 0.9800 . ?
C23 C24 1.524(3) . ?
C23 C25 1.532(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26 0.9800 . ?
C26 C27 1.524(3) . ?
C26 C28 1.537(3) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.402(3) . ?
C29 C34 1.401(3) . ?
C30 C31 1.396(3) . ?
C30 C35 1.524(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.378(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.383(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.393(3) . ?
C34 C38 1.524(3) . ?
C35 H35 0.9800 . ?
C35 C36 1.521(3) . ?
C35 C37 1.526(3) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38 0.9800 . ?
C38 C39 1.524(3) . ?
C38 C40 1.524(3) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.395(3) . ?
C41 C46 1.393(3) . ?
C42 H42 0.9300 . ?
C42 C43 1.385(3) . ?
C43 H43 0.9300 . ?
C43 C44 1.378(3) . ?
C44 H44 0.9300 . ?
C44 C45 1.390(3) . ?
C45 H45 0.9300 . ?
C45 C46 1.388(3) . ?
C46 H46 0.9300 . ?
C47 C48 1.396(3) . ?
C47 C52 1.389(3) . ?
C48 H48 0.9300 . ?
C48 C49 1.385(3) . ?
C49 H49 0.9300 . ?
C49 C50 1.383(3) . ?
C50 H50 0.9300 . ?
C50 C51 1.384(3) . ?
C51 H51 0.9300 . ?
C51 C52 1.393(3) . ?
C52 H52 0.9300 . ?
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
P1 C2 C3 N2 156.44(15) . . . . ?
P1 C2 C3 C4 -21.9(3) . . . . ?
P1 C41 C42 C43 -171.34(16) . . . . ?
P1 C41 C46 C45 171.07(16) . . . . ?
P1 C47 C48 C49 -176.74(17) . . . . ?
P1 C47 C52 C51 175.62(16) . . . . ?
N1 C1 C11 C12 40.6(3) . . . . ?
N1 C1 C11 C16 -135.3(2) . . . . ?
N1 C2 C3 N2 -5.39(18) . . . . ?
N1 C2 C3 C4 176.30(17) . . . . ?
N1 C17 C18 C19 -177.02(16) . . . . ?
N1 C17 C18 C23 3.5(3) . . . . ?
N1 C17 C22 C21 178.31(17) . . . . ?
N1 C17 C22 C26 -0.4(3) . . . . ?
N2 C1 C11 C12 -145.51(19) . . . . ?
N2 C1 C11 C16 38.5(3) . . . . ?
N2 C3 C4 C5 -5.8(4) . . . . ?
N2 C29 C30 C31 177.55(17) . . . . ?
N2 C29 C30 C35 -2.8(3) . . . . ?
N2 C29 C34 C33 -177.23(17) . . . . ?
N2 C29 C34 C38 6.9(3) . . . . ?
C1 N1 C2 P1 -160.91(13) . . . . ?
C1 N1 C2 C3 4.3(2) . . . . ?
C1 N1 C17 C18 -107.5(2) . . . . ?
C1 N1 C17 C22 76.0(2) . . . . ?
C1 N2 C3 C2 4.96(19) . . . . ?
C1 N2 C3 C4 -176.88(19) . . . . ?
C1 N2 C29 C30 -112.7(2) . . . . ?
C1 N2 C29 C34 66.4(2) . . . . ?
C1 C11 C12 C13 -174.96(18) . . . . ?
C1 C11 C16 C15 173.45(18) . . . . ?
C2 P1 C41 C42 151.51(15) . . . . ?
C2 P1 C41 C46 -21.18(19) . . . . ?
C2 P1 C47 C48 -51.34(17) . . . . ?
C2 P1 C47 C52 133.93(17) . . . . ?
C2 N1 C1 N2 -1.2(2) . . . . ?
C2 N1 C1 C11 173.69(16) . . . . ?
C2 N1 C17 C18 76.0(2) . . . . ?
C2 N1 C17 C22 -100.5(2) . . . . ?
C2 C3 C4 C5 172.0(2) . . . . ?
C3 N2 C1 N1 -2.49(19) . . . . ?
C3 N2 C1 C11 -177.26(17) . . . . ?
C3 N2 C29 C30 72.3(2) . . . . ?
C3 N2 C29 C34 -108.6(2) . . . . ?
C3 C4 C5 C6 38.1(4) . . . . ?
C3 C4 C5 C10 -145.5(2) . . . . ?
C4 C5 C6 C7 178.86(19) . . . . ?
C4 C5 C10 C9 -178.4(2) . . . . ?
C5 C6 C7 C8 -1.3(3) . . . . ?
C6 C5 C10 C9 -1.5(3) . . . . ?
C6 C7 C8 C9 -0.8(3) . . . . ?
C7 C8 C9 C10 1.7(3) . . . . ?
C8 C9 C10 C5 -0.5(3) . . . . ?
C10 C5 C6 C7 2.4(3) . . . . ?
C11 C12 C13 C14 1.6(3) . . . . ?
C12 C11 C16 C15 -2.6(3) . . . . ?
C12 C13 C14 C15 -2.8(3) . . . . ?
C13 C14 C15 C16 1.2(3) . . . . ?
C14 C15 C16 C11 1.5(3) . . . . ?
C16 C11 C12 C13 1.1(3) . . . . ?
C17 N1 C1 N2 -178.02(16) . . . . ?
C17 N1 C1 C11 -3.1(3) . . . . ?
C17 N1 C2 P1 16.1(2) . . . . ?
C17 N1 C2 C3 -178.69(15) . . . . ?
C17 C18 C19 C20 -0.4(3) . . . . ?
C17 C18 C23 C24 -139.75(19) . . . . ?
C17 C18 C23 C25 96.9(2) . . . . ?
C17 C22 C26 C27 -119.7(2) . . . . ?
C17 C22 C26 C28 116.5(2) . . . . ?
C18 C17 C22 C21 2.0(3) . . . . ?
C18 C17 C22 C26 -176.65(18) . . . . ?
C18 C19 C20 C21 0.1(3) . . . . ?
C19 C18 C23 C24 40.8(3) . . . . ?
C19 C18 C23 C25 -82.6(2) . . . . ?
C19 C20 C21 C22 1.3(3) . . . . ?
C20 C21 C22 C17 -2.3(3) . . . . ?
C20 C21 C22 C26 176.46(19) . . . . ?
C21 C22 C26 C27 61.6(2) . . . . ?
C21 C22 C26 C28 -62.2(2) . . . . ?
C22 C17 C18 C19 -0.7(3) . . . . ?
C22 C17 C18 C23 179.80(18) . . . . ?
C23 C18 C19 C20 179.11(19) . . . . ?
C29 N2 C1 N1 -178.22(15) . . . . ?
C29 N2 C1 C11 7.0(3) . . . . ?
C29 N2 C3 C2 -179.54(16) . . . . ?
C29 N2 C3 C4 -1.4(3) . . . . ?
C29 C30 C31 C32 -0.1(3) . . . . ?
C29 C30 C35 C36 94.6(3) . . . . ?
C29 C30 C35 C37 -141.04(19) . . . . ?
C29 C34 C38 C39 -151.0(2) . . . . ?
C29 C34 C38 C40 83.3(2) . . . . ?
C30 C29 C34 C33 1.8(3) . . . . ?
C30 C29 C34 C38 -174.13(18) . . . . ?
C30 C31 C32 C33 1.3(3) . . . . ?
C31 C30 C35 C36 -85.7(3) . . . . ?
C31 C30 C35 C37 38.6(3) . . . . ?
C31 C32 C33 C34 -0.9(3) . . . . ?
C32 C33 C34 C29 -0.6(3) . . . . ?
C32 C33 C34 C38 175.38(19) . . . . ?
C33 C34 C38 C39 33.2(3) . . . . ?
C33 C34 C38 C40 -92.5(2) . . . . ?
C34 C29 C30 C31 -1.4(3) . . . . ?
C34 C29 C30 C35 178.21(18) . . . . ?
C35 C30 C31 C32 -179.77(19) . . . . ?
C41 P1 C2 N1 -115.74(14) . . . . ?
C41 P1 C2 C3 84.0(2) . . . . ?
C41 P1 C47 C48 -160.77(16) . . . . ?
C41 P1 C47 C52 24.50(19) . . . . ?
C41 C42 C43 C44 0.0(3) . . . . ?
C42 C41 C46 C45 -1.5(3) . . . . ?
C42 C43 C44 C45 -2.0(3) . . . . ?
C43 C44 C45 C46 2.3(3) . . . . ?
C44 C45 C46 C41 -0.5(3) . . . . ?
C46 C41 C42 C43 1.8(3) . . . . ?
C47 P1 C2 N1 136.06(14) . . . . ?
C47 P1 C2 C3 -24.2(2) . . . . ?
C47 P1 C41 C42 -102.32(16) . . . . ?
C47 P1 C41 C46 84.99(18) . . . . ?
C47 C48 C49 C50 0.9(3) . . . . ?
C48 C47 C52 C51 0.9(3) . . . . ?
C48 C49 C50 C51 0.8(4) . . . . ?
C49 C50 C51 C52 -1.7(4) . . . . ?
C50 C51 C52 C47 0.8(3) . . . . ?
C52 C47 C48 C49 -1.8(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
-1.0000 -0.0000 -1.0000 -0.0281 -0.1160 -0.1300
1.0000 0.0000 1.0000 0.0281 0.1160 0.1300
-4.0423 -0.7039 10.4268 -0.9996 0.0257 -0.0091
4.0423 0.7039 -10.4268 0.9996 -0.0257 0.0091
-2.6035 4.6462 -1.9970 -0.0263 0.0044 -0.9996
2.6035 -4.6462 1.9970 0.0263 -0.0044 0.9996
