#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:48:58 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228942 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/11/7231136.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_7231136
loop_
_publ_author_name
'Wong, Lawrence W.-Y.'
'Tam, Gemma S.-S.'
'Chen, Xiaoyan'
'So, Frederick T.-K.'
'Soecipto, Aristyo'
'Sheong, Fu Kit'
'Sung, Herman H.-Y.'
'Lin, Zhenyang'
'Williams, Ian D.'
_publ_section_title
;
 A chiral spiroborate anion from diphenyl-l-tartramide
 [B{l-Tar(NHPh)2}2]−applied to some challenging resolutions
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4831
_journal_paper_doi               10.1039/C8CE00855H
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C16 H14 B0.5 N2 O4), 2(H2 N0.5)'
_chemical_formula_sum            'C32 H32 B N5 O8'
_chemical_formula_weight         625.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-21
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-05-22 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.965(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.9663(9)
_cell_length_b                   13.3119(4)
_cell_length_c                   7.0955(3)
_cell_measurement_reflns_used    3690
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.0130
_cell_measurement_theta_min      5.3590
_cell_volume                     2917.91(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     57.00 140.00   1.00   45.00    --  110.57 -77.00  60.00   83
  2  ω    -86.00  13.00   1.00   18.00    --  -40.20  19.00  90.00   99
  3  ω    -95.00  -2.00   1.00   18.00    --  -40.20 125.00  60.00   93
  4  ω   -100.00 -22.00   1.00   18.00    --  -40.20 -37.00-120.00   78
  5  ω   -122.00   6.00   1.00   18.00    --  -40.20 -19.00  30.00  128
  6  ω     99.00 176.00   1.00   45.00    --  110.57  61.00  30.00   77
  7  ω     83.00 178.00   1.00   45.00    --  110.57  45.00  90.00   95
  8  ω     36.00 119.00   1.00   45.00    --  110.57 -45.00   0.00   83
  9  ω     33.00 115.00   1.00   45.00    --  110.57-111.00  30.00   82
 10  ω     77.00 178.00   1.00   45.00    --  110.57  77.00 -90.00  101
 11  ω     28.00 172.00   1.00   45.00    --  110.57 -15.00 -90.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0203673000
_diffrn_orient_matrix_UB_12      0.0271677000
_diffrn_orient_matrix_UB_13      0.1978124000
_diffrn_orient_matrix_UB_21      -0.0265454000
_diffrn_orient_matrix_UB_22      0.0979498000
_diffrn_orient_matrix_UB_23      -0.0034425000
_diffrn_orient_matrix_UB_31      -0.0369712000
_diffrn_orient_matrix_UB_32      -0.0552735000
_diffrn_orient_matrix_UB_33      0.0908602000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8914
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         75.735
_diffrn_reflns_theta_min         3.615
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       needle
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.09(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         8914
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0751P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                7836
_reflns_number_total             8914
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00855h2.cif
_cod_data_source_block           gem57d_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7231133--7231140.cif.'
_cod_original_cell_volume        2917.92(17)
_cod_database_code               7231136
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C20 N2 O6'
_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   0.975
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4990(14)
 0.5010(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3.a Riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B)
3.b Ternary CH refined with riding coordinates:
 C12(H12), C13(H13), C22(H22), C23(H23)
3.c Aromatic/amide H refined with riding coordinates:
 N11(H11), N14(H14), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), N21(H21), N24(H24), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66)
;
_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 1.508
_oxdiff_exptl_absorpt_empirical_full_min 0.697
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.9842° 
 around [-0.29 -0.00 0.96] (reciprocal) or [-0.00 -0.00 1.00] (direct)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, 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
O11 O 0.36365(9) 0.1295(2) 0.4231(5) 0.0227(6) Uani 1 1 d . . .
O12 O 0.47363(8) 0.2011(2) 0.3632(4) 0.0169(6) Uani 1 1 d . . .
O13 O 0.46859(8) 0.3274(2) 0.5891(4) 0.0161(6) Uani 1 1 d . . .
O14 O 0.40923(9) 0.4686(2) 0.4952(4) 0.0197(6) Uani 1 1 d . . .
N11 N 0.42825(11) 0.0440(3) 0.4587(5) 0.0181(7) Uani 1 1 d . . .
H11 H 0.4563 0.0554 0.4653 0.022 Uiso 1 1 calc R . .
N14 N 0.35379(11) 0.3540(3) 0.4767(6) 0.0221(8) Uani 1 1 d . . .
H14 H 0.3490 0.2889 0.4715 0.027 Uiso 1 1 calc R . .
C11 C 0.40332(12) 0.1245(3) 0.4201(6) 0.0177(8) Uani 1 1 d . . .
C12 C 0.42893(12) 0.2198(3) 0.3778(6) 0.0159(8) Uani 1 1 d . . .
H12 H 0.4163 0.2521 0.2593 0.019 Uiso 1 1 calc R . .
C13 C 0.42627(12) 0.2929(3) 0.5472(6) 0.0161(8) Uani 1 1 d . . .
H13 H 0.4163 0.2552 0.6582 0.019 Uiso 1 1 calc R . .
C14 C 0.39582(13) 0.3816(3) 0.5025(6) 0.0171(8) Uani 1 1 d . . .
C31 C 0.41612(13) -0.0573(3) 0.4906(6) 0.0178(8) Uani 1 1 d . . .
C32 C 0.44779(13) -0.1206(3) 0.5733(6) 0.0202(8) Uani 1 1 d . . .
H32 H 0.4752 -0.0942 0.6159 0.024 Uiso 1 1 calc R . .
C33 C 0.43942(14) -0.2224(3) 0.5937(6) 0.0235(9) Uani 1 1 d . . .
H33 H 0.4611 -0.2656 0.6500 0.028 Uiso 1 1 calc R . .
C34 C 0.39939(15) -0.2607(3) 0.5315(7) 0.0255(10) Uani 1 1 d . . .
H34 H 0.3936 -0.3304 0.5435 0.031 Uiso 1 1 calc R . .
C35 C 0.36777(14) -0.1972(3) 0.4520(6) 0.0241(9) Uani 1 1 d . . .
H35 H 0.3402 -0.2238 0.4118 0.029 Uiso 1 1 calc R . .
C36 C 0.37563(14) -0.0952(3) 0.4300(6) 0.0203(9) Uani 1 1 d . . .
H36 H 0.3538 -0.0522 0.3747 0.024 Uiso 1 1 calc R . .
C41 C 0.31645(13) 0.4157(3) 0.4571(6) 0.0216(9) Uani 1 1 d . . .
C42 C 0.31761(15) 0.5199(4) 0.4604(9) 0.0347(13) Uani 1 1 d . . .
H42 H 0.3446 0.5543 0.4685 0.042 Uiso 1 1 calc R . .
C43 C 0.27910(16) 0.5736(4) 0.4516(10) 0.0382(13) Uani 1 1 d . . .
H43 H 0.2800 0.6449 0.4553 0.046 Uiso 1 1 calc R . .
C44 C 0.23971(15) 0.5256(4) 0.4377(7) 0.0278(11) Uani 1 1 d . . .
H44 H 0.2136 0.5632 0.4337 0.033 Uiso 1 1 calc R . .
C45 C 0.23858(14) 0.4220(4) 0.4296(7) 0.0289(11) Uani 1 1 d . . .
H45 H 0.2115 0.3884 0.4171 0.035 Uiso 1 1 calc R . .
C46 C 0.27677(14) 0.3663(4) 0.4396(7) 0.0238(9) Uani 1 1 d . . .
H46 H 0.2757 0.2951 0.4345 0.029 Uiso 1 1 calc R . .
B1 B 0.5000 0.2647(5) 0.5000 0.0165(13) Uani 1 2 d S T P
O21 O 0.59001(9) 0.3568(2) 0.0286(5) 0.0192(6) Uani 1 1 d . . .
O22 O 0.53258(8) 0.4997(2) 0.1002(4) 0.0163(6) Uani 1 1 d . . .
O23 O 0.52478(8) 0.6253(2) -0.1288(4) 0.0168(6) Uani 1 1 d . . .
O24 O 0.63582(9) 0.6894(2) -0.0127(5) 0.0224(6) Uani 1 1 d . . .
N2 N 0.5000 0.3018(4) 0.0000 0.0179(10) Uani 1 2 d S T P
H2A H 0.4815 0.3435 -0.0181 0.43(14) Uiso 1 1 d R . .
H2B H 0.5013 0.2655 -0.1050 0.12(4) Uiso 1 1 d R . .
N21 N 0.64608(11) 0.4688(3) 0.0366(6) 0.0212(8) Uani 1 1 d . . .
H21 H 0.6512 0.5338 0.0338 0.025 Uiso 1 1 calc R . .
N24 N 0.57425(10) 0.7843(3) -0.0591(5) 0.0174(7) Uani 1 1 d . . .
H24 H 0.5468 0.7787 -0.0996 0.021 Uiso 1 1 calc R . .
C21 C 0.60416(13) 0.4423(3) 0.0420(6) 0.0179(8) Uani 1 1 d . . .
C22 C 0.57465(12) 0.5326(3) 0.0733(6) 0.0161(8) Uani 1 1 d . . .
H22 H 0.5862 0.5708 0.1871 0.019 Uiso 1 1 calc R . .
C23 C 0.56967(11) 0.6050(3) -0.1002(6) 0.0162(8) Uani 1 1 d . . .
H23 H 0.5801 0.5711 -0.2143 0.019 Uiso 1 1 calc R . .
C24 C 0.59693(12) 0.6983(3) -0.0536(6) 0.0173(8) Uani 1 1 d . . .
C51 C 0.68302(13) 0.4057(3) 0.0347(6) 0.0219(9) Uani 1 1 d . . .
C52 C 0.68080(14) 0.3028(4) 0.0029(8) 0.0273(10) Uani 1 1 d . . .
H52 H 0.6536 0.2711 -0.0247 0.033 Uiso 1 1 calc R . .
C53 C 0.71884(16) 0.2466(4) 0.0119(9) 0.0340(12) Uani 1 1 d . . .
H53 H 0.7173 0.1761 -0.0085 0.041 Uiso 1 1 calc R . .
C54 C 0.75854(15) 0.2913(4) 0.0497(8) 0.0333(12) Uani 1 1 d . . .
H54 H 0.7843 0.2523 0.0561 0.040 Uiso 1 1 calc R . .
C55 C 0.76041(15) 0.3949(5) 0.0785(7) 0.0299(11) Uani 1 1 d . . .
H55 H 0.7877 0.4268 0.1033 0.036 Uiso 1 1 calc R . .
C56 C 0.72308(14) 0.4514(4) 0.0712(7) 0.0253(10) Uani 1 1 d . . .
H56 H 0.7247 0.5219 0.0912 0.030 Uiso 1 1 calc R . .
C61 C 0.58793(14) 0.8825(3) -0.0096(6) 0.0190(8) Uani 1 1 d . . .
C62 C 0.55737(14) 0.9585(3) -0.0365(7) 0.0233(9) Uani 1 1 d . . .
H62 H 0.5292 0.9433 -0.0906 0.028 Uiso 1 1 calc R . .
C63 C 0.56780(16) 1.0570(3) 0.0153(7) 0.0293(10) Uani 1 1 d . . .
H63 H 0.5466 1.1084 -0.0007 0.035 Uiso 1 1 calc R . .
C64 C 0.60905(16) 1.0797(4) 0.0901(7) 0.0281(10) Uani 1 1 d . . .
H64 H 0.6163 1.1468 0.1255 0.034 Uiso 1 1 calc R . .
C65 C 0.63947(15) 1.0047(4) 0.1129(7) 0.0273(10) Uani 1 1 d . . .
H65 H 0.6679 1.0210 0.1623 0.033 Uiso 1 1 calc R . .
C66 C 0.62958(14) 0.9050(3) 0.0653(6) 0.0206(9) Uani 1 1 d . . .
H66 H 0.6508 0.8538 0.0835 0.025 Uiso 1 1 calc R . .
B2 B 0.5000 0.5624(5) 0.0000 0.0159(13) Uani 1 2 d S T P
N1 N 0.5000 0.5283(4) 0.5000 0.0173(10) Uani 1 2 d S T P
H1A H 0.5186 0.4922 0.4741 0.039(17) Uiso 1 1 d R . .
H1B H 0.4984 0.5628 0.3803 0.05(2) Uiso 1 1 d 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'
B B 0.0090 0.0039 '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'
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
C12 O12 B1 110.3(3) . .
C13 O13 B1 111.2(3) . .
C11 N11 C31 129.6(3) . .
C14 N14 C41 128.8(4) . .
O11 C11 N11 127.0(4) . .
O11 C11 C12 119.2(4) . .
N11 C11 C12 113.7(3) . .
O12 C12 C11 112.9(3) . .
O12 C12 C13 105.7(3) . .
C11 C12 C13 108.1(3) . .
O13 C13 C12 105.7(3) . .
O13 C13 C14 110.1(3) . .
C14 C13 C12 112.8(3) . .
O14 C14 N14 125.0(4) . .
O14 C14 C13 122.0(4) . .
N14 C14 C13 113.0(4) . .
C32 C31 N11 117.1(4) . .
C36 C31 N11 122.5(4) . .
C36 C31 C32 120.2(4) . .
C33 C32 C31 120.3(4) . .
C34 C33 C32 119.7(4) . .
C33 C34 C35 119.9(4) . .
C34 C35 C36 121.2(4) . .
C35 C36 C31 118.7(4) . .
C42 C41 N14 123.9(4) . .
C42 C41 C46 119.7(4) . .
C46 C41 N14 116.4(4) . .
C43 C42 C41 119.5(5) . .
C44 C43 C42 121.3(5) . .
C43 C44 C45 119.1(5) . .
C44 C45 C46 120.7(4) . .
C41 C46 C45 119.6(4) . .
O12 B1 O12 110.6(5) 2_656 .
O13 B1 O12 104.85(14) 2_656 2_656
O13 B1 O12 113.27(15) 2_656 .
O13 B1 O12 104.85(14) . .
O13 B1 O12 113.27(15) . 2_656
O13 B1 O13 110.2(5) 2_656 .
C22 O22 B2 112.0(3) . .
C23 O23 B2 110.3(3) . .
C21 N21 C51 128.6(4) . .
C24 N24 C61 129.4(3) . .
O21 C21 N21 125.6(4) . .
O21 C21 C22 121.8(4) . .
N21 C21 C22 112.6(4) . .
O22 C22 C21 110.2(3) . .
O22 C22 C23 105.0(3) . .
C21 C22 C23 113.4(3) . .
O23 C23 C22 105.8(3) . .
O23 C23 C24 113.5(3) . .
C24 C23 C22 108.0(3) . .
O24 C24 N24 126.4(4) . .
O24 C24 C23 119.5(4) . .
N24 C24 C23 114.1(3) . .
C52 C51 N21 123.6(4) . .
C56 C51 N21 116.7(4) . .
C56 C51 C52 119.7(4) . .
C51 C52 C53 119.3(4) . .
C54 C53 C52 121.2(5) . .
C53 C54 C55 118.9(4) . .
C56 C55 C54 120.5(5) . .
C55 C56 C51 120.3(5) . .
C62 C61 N24 116.8(4) . .
C62 C61 C66 120.0(4) . .
C66 C61 N24 123.2(4) . .
C61 C62 C63 120.4(4) . .
C64 C63 C62 119.9(4) . .
C65 C64 C63 119.6(4) . .
C64 C65 C66 121.6(4) . .
C61 C66 C65 118.5(4) . .
O22 B2 O22 110.1(5) 2_655 .
O22 B2 O23 104.62(14) 2_655 2_655
O22 B2 O23 113.00(16) . 2_655
O22 B2 O23 113.00(16) 2_655 .
O22 B2 O23 104.62(14) . .
O23 B2 O23 111.7(5) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O11 C11 1.232(5) .
O12 C12 1.417(4) .
O12 B1 1.489(4) .
O13 C13 1.401(4) .
O13 B1 1.459(5) .
O14 C14 1.232(5) .
N11 C11 1.338(5) .
N11 C31 1.422(5) .
N14 C14 1.353(5) .
N14 C41 1.417(5) .
C11 C12 1.536(5) .
C12 C13 1.553(6) .
C13 C14 1.531(5) .
C31 C32 1.392(6) .
C31 C36 1.392(6) .
C32 C33 1.389(6) .
C33 C34 1.384(7) .
C34 C35 1.384(7) .
C35 C36 1.390(6) .
C41 C42 1.388(7) .
C41 C46 1.391(6) .
C42 C43 1.388(7) .
C43 C44 1.374(7) .
C44 C45 1.380(7) .
C45 C46 1.393(6) .
B1 O12 1.489(4) 2_656
B1 O13 1.459(5) 2_656
O21 C21 1.221(5) .
O22 C22 1.400(5) .
O22 B2 1.456(5) .
O23 C23 1.417(4) .
O23 B2 1.490(5) .
O24 C24 1.225(5) .
N21 C21 1.348(5) .
N21 C51 1.420(5) .
N24 C24 1.343(5) .
N24 C61 1.411(5) .
C21 C22 1.535(6) .
C22 C23 1.563(5) .
C23 C24 1.525(5) .
C51 C52 1.389(7) .
C51 C56 1.389(6) .
C52 C53 1.393(6) .
C53 C54 1.375(8) .
C54 C55 1.395(8) .
C55 C56 1.376(7) .
C61 C62 1.389(6) .
C61 C66 1.393(6) .
C62 C63 1.393(7) .
C63 C64 1.383(7) .
C64 C65 1.375(7) .
C65 C66 1.398(6) .
B2 O22 1.456(5) 2_655
B2 O23 1.490(5) 2_655
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H11 O12 0.88 2.15 2.634(4) 114.0 .
N14 H14 O11 0.88 2.20 3.031(5) 156.9 .
N2 H2A O21 0.80 2.22 2.875(3) 139.5 2_655
N2 H2A O22 0.80 2.20 2.893(6) 145.6 2_655
N2 H2B O12 0.89 2.21 3.065(4) 160.3 2_655
N2 H2B O13 0.89 2.47 3.028(3) 121.0 1_554
N21 H21 O24 0.88 2.15 2.972(5) 156.0 .
N24 H24 O23 0.88 2.16 2.640(4) 113.9 .
N1 H1A O13 0.78 2.28 2.929(5) 141.2 2_656
N1 H1A O14 0.78 2.25 2.919(3) 143.7 2_656
N1 H1B O22 0.96 2.46 3.099(3) 123.3 .
N1 H1B O23 0.96 2.05 2.985(4) 162.3 2_655
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_4
O11 C11 C12 O12 -175.0(4) .
O11 C11 C12 C13 68.5(5) .
O12 C12 C13 O13 12.6(4) .
O12 C12 C13 C14 133.1(3) .
O13 C13 C14 O14 4.2(6) .
O13 C13 C14 N14 -174.6(4) .
N11 C11 C12 O12 7.9(5) .
N11 C11 C12 C13 -108.7(4) .
N11 C31 C32 C33 -174.4(4) .
N11 C31 C36 C35 174.3(4) .
N14 C41 C42 C43 -176.1(5) .
N14 C41 C46 C45 176.7(4) .
C11 N11 C31 C32 -164.5(4) .
C11 N11 C31 C36 20.4(7) .
C11 C12 C13 O13 133.8(3) .
C11 C12 C13 C14 -105.8(4) .
C12 O12 B1 O12 118.9(3) 2_656
C12 O12 B1 O13 -123.7(3) 2_656
C12 O12 B1 O13 -3.5(4) .
C12 C13 C14 O14 -113.7(4) .
C12 C13 C14 N14 67.5(4) .
C13 O13 B1 O12 12.2(4) .
C13 O13 B1 O12 -108.4(4) 2_656
C13 O13 B1 O13 134.4(3) 2_656
C14 N14 C41 C42 0.5(8) .
C14 N14 C41 C46 -177.5(5) .
C31 N11 C11 O11 8.1(8) .
C31 N11 C11 C12 -174.9(4) .
C31 C32 C33 C34 -0.1(7) .
C32 C31 C36 C35 -0.6(6) .
C32 C33 C34 C35 -0.9(7) .
C33 C34 C35 C36 1.1(7) .
C34 C35 C36 C31 -0.3(7) .
C36 C31 C32 C33 0.8(7) .
C41 N14 C14 O14 -7.4(8) .
C41 N14 C14 C13 171.3(4) .
C41 C42 C43 C44 -0.7(10) .
C42 C41 C46 C45 -1.4(7) .
C42 C43 C44 C45 -0.9(9) .
C43 C44 C45 C46 1.4(8) .
C44 C45 C46 C41 -0.3(7) .
C46 C41 C42 C43 1.9(8) .
B1 O12 C12 C11 -123.3(4) .
B1 O12 C12 C13 -5.4(4) .
B1 O13 C13 C12 -15.4(4) .
B1 O13 C13 C14 -137.6(3) .
O21 C21 C22 O22 5.5(6) .
O21 C21 C22 C23 -111.8(4) .
O22 C22 C23 O23 13.3(4) .
O22 C22 C23 C24 135.1(3) .
O23 C23 C24 O24 174.8(4) .
O23 C23 C24 N24 -3.9(5) .
N21 C21 C22 O22 -173.0(3) .
N21 C21 C22 C23 69.8(5) .
N21 C51 C52 C53 -177.3(5) .
N21 C51 C56 C55 177.8(4) .
N24 C61 C62 C63 177.6(4) .
N24 C61 C66 C65 -178.8(4) .
C21 N21 C51 C52 12.6(7) .
C21 N21 C51 C56 -166.0(5) .
C21 C22 C23 O23 133.5(3) .
C21 C22 C23 C24 -104.6(4) .
C22 O22 B2 O22 133.9(3) 2_655
C22 O22 B2 O23 12.2(4) .
C22 O22 B2 O23 -109.6(4) 2_655
C22 C23 C24 O24 57.9(5) .
C22 C23 C24 N24 -120.9(4) .
C23 O23 B2 O22 -122.6(3) 2_655
C23 O23 B2 O22 -2.9(4) .
C23 O23 B2 O23 119.7(3) 2_655
C24 N24 C61 C62 177.7(4) .
C24 N24 C61 C66 -3.1(7) .
C51 N21 C21 O21 -7.3(7) .
C51 N21 C21 C22 171.1(4) .
C51 C52 C53 C54 -0.7(8) .
C52 C51 C56 C55 -0.9(7) .
C52 C53 C54 C55 -0.3(8) .
C53 C54 C55 C56 0.7(8) .
C54 C55 C56 C51 -0.1(7) .
C56 C51 C52 C53 1.3(8) .
C61 N24 C24 O24 -4.4(7) .
C61 N24 C24 C23 174.2(4) .
C61 C62 C63 C64 1.4(7) .
C62 C61 C66 C65 0.4(7) .
C62 C63 C64 C65 -0.1(7) .
C63 C64 C65 C66 -1.1(7) .
C64 C65 C66 C61 0.9(7) .
C66 C61 C62 C63 -1.6(7) .
B2 O22 C22 C21 -138.1(3) .
B2 O22 C22 C23 -15.8(4) .
B2 O23 C23 C22 -6.2(4) .
B2 O23 C23 C24 -124.4(4) .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4990(14) 4694 4388 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.5010(14) 4672 4388 nmt -0.9998 0.0024 -0.6162 -0.0001 -0.9999 -0.0001
-0.0000 -0.0001 1.0000
