#------------------------------------------------------------------------------
#$Date: 2021-11-16 01:02:25 +0200 (Tue, 16 Nov 2021) $
#$Revision: 270663 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/92/7129250.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_7129250
loop_
_publ_author_name
'Hill, Anthony'
'Frogley, Benjamin'
'Welsh, Steven S.'
_publ_section_title
;
 Bimetallic ethynylanthracenyl functionalised carbynes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06142A
_journal_year                    2021
_chemical_formula_moiety         'C74 H64 B2 N12 O4 W2'
_chemical_formula_sum            'C74 H64 B2 N12 O4 W2'
_chemical_formula_weight         1574.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-21 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.982(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.7180(16)
_cell_length_b                   9.4131(4)
_cell_length_c                   18.4744(16)
_cell_measurement_reflns_used    5397
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.3750
_cell_measurement_theta_min      3.9670
_cell_volume                     3637.1(5)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.814
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  40.00   1.00   48.00    --   12.97 -77.00 -60.00   82
  2  ω     51.00  85.00   1.00   48.00    --   12.97 178.00  90.00   34
  3  ω    -39.00  42.00   1.00   48.00    --   12.97 -19.00  30.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0283781000
_diffrn_orient_matrix_UB_12      0.0363363000
_diffrn_orient_matrix_UB_13      0.0235891000
_diffrn_orient_matrix_UB_21      -0.0185059000
_diffrn_orient_matrix_UB_22      0.0522834000
_diffrn_orient_matrix_UB_23      0.0091180000
_diffrn_orient_matrix_UB_31      0.0016061000
_diffrn_orient_matrix_UB_32      -0.0402490000
_diffrn_orient_matrix_UB_33      0.0331990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.814
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14153
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.215
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.033
_refine_diff_density_max         3.071
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0454
_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)+(0.0423P)²+3.5084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5551
_reflns_number_total             7366
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc06142a2.cif
_cod_data_source_block           Compound_8
_cod_database_code               7129250
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C74 H60 B2 N12 O4 W2'
_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.
;
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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 Aromatic/amide H refined with riding coordinates:
 C25(H25), C6(H6), C16(H16), C30(H30), C14(H14), C7(H7), C13(H13), C21(H21),
 C15(H15), C22(H22), C9(H9), C8(H8), C35(H35)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C33(H33A,H33B,
 H33C), C32(H32A,H32B,H32C), C37(H37A,H37B,H37C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_ins_header
;
TITL BF125D2a_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  22.717998   9.413102  18.474442  90.0000 112.9821  90.0000
ZERR    2.00   0.001641   0.000410   0.001585   0.0000   0.0097   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O W
UNIT 148.00 120.00 4.00 24.00 8.00 4.00
TREF
HKLF 4
END
;
_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 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.786
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
W1 W 0.17215(2) 0.45768(2) 0.26311(2) 0.03723(10) Uani 1 1 d . . . . .
O2 O 0.0645(2) 0.4870(5) 0.0940(3) 0.0543(12) Uani 1 1 d . . . . .
N1 N 0.1015(2) 0.3519(5) 0.3084(3) 0.0343(11) Uani 1 1 d . . . . .
N3 N 0.1448(2) 0.6480(5) 0.3110(3) 0.0355(11) Uani 1 1 d . . . . .
N2 N 0.1033(2) 0.3898(5) 0.3806(3) 0.0373(11) Uani 1 1 d . . . . .
N4 N 0.1372(2) 0.6439(5) 0.3816(3) 0.0431(12) Uani 1 1 d . . . . .
C3 C 0.1033(3) 0.4749(6) 0.1557(4) 0.0387(14) Uani 1 1 d . . . . .
N5 N 0.2379(2) 0.4299(5) 0.3865(3) 0.0483(13) Uani 1 1 d . . . . .
C1 C 0.2251(2) 0.5351(5) 0.2211(3) 0.0336(13) Uani 1 1 d . . . . .
N6 N 0.2196(2) 0.4561(5) 0.4481(3) 0.0495(13) Uani 1 1 d . . . . .
O1 O 0.2075(3) 0.1578(5) 0.2190(4) 0.0833(18) Uani 1 1 d . . . . .
C2 C 0.1937(3) 0.2670(7) 0.2339(4) 0.0570(19) Uani 1 1 d . . . . .
C4 C 0.2649(3) 0.5994(6) 0.1854(3) 0.0372(14) Uani 1 1 d . . . . .
C26 C 0.0613(3) 0.3093(6) 0.3977(4) 0.0415(15) Uani 1 1 d . . . . .
C28 C 0.1324(3) 0.8295(6) 0.2069(4) 0.0494(16) Uani 1 1 d . . . . .
H28A H 0.150770 0.756066 0.186293 0.074 Uiso 1 1 calc GR . . . .
H28B H 0.157719 0.914197 0.215066 0.074 Uiso 1 1 calc GR . . . .
H28C H 0.089624 0.848757 0.170288 0.074 Uiso 1 1 calc GR . . . .
C24 C 0.0575(3) 0.2498(6) 0.2800(4) 0.0414(15) Uani 1 1 d . . . . .
C17 C 0.3070(3) 0.7107(6) 0.2259(3) 0.0357(13) Uani 1 1 d . . . . .
C25 C 0.0319(3) 0.2208(6) 0.3355(4) 0.0471(16) Uani 1 1 d . . . . .
H25 H 0.000571 0.153772 0.331036 0.056 Uiso 1 1 calc R . . . .
C6 C 0.2199(3) 0.4476(7) 0.0673(4) 0.0484(16) Uani 1 1 d . . . . .
H6 H 0.194020 0.402351 0.088735 0.058 Uiso 1 1 calc R . . . .
C29 C 0.1310(3) 0.7817(6) 0.2838(4) 0.0407(14) Uani 1 1 d . . . . .
C10 C 0.3013(3) 0.6211(7) 0.0761(4) 0.0461(16) Uani 1 1 d . . . . .
C5 C 0.2621(3) 0.5538(6) 0.1109(4) 0.0410(14) Uani 1 1 d . . . . .
C31 C 0.1183(3) 0.7709(6) 0.3972(4) 0.0465(15) Uani 1 1 d . . . . .
C12 C 0.3494(3) 0.7717(6) 0.1938(4) 0.0407(14) Uani 1 1 d . . . . .
C16 C 0.3079(3) 0.7691(6) 0.2968(3) 0.0422(15) Uani 1 1 d . . . . .
H16 H 0.280987 0.730933 0.318986 0.051 Uiso 1 1 calc R . . . .
C30 C 0.1135(3) 0.8598(7) 0.3360(4) 0.0512(16) Uani 1 1 d . . . . .
H30 H 0.100939 0.954570 0.330648 0.061 Uiso 1 1 calc R . . . .
C14 C 0.3890(3) 0.9380(7) 0.3025(4) 0.0482(16) Uani 1 1 d . . . . .
H14 H 0.415671 1.013139 0.327856 0.058 Uiso 1 1 calc R . . . .
C11 C 0.3462(3) 0.7263(7) 0.1192(3) 0.0443(15) Uani 1 1 d . . . . .
C23 C 0.0407(3) 0.1829(7) 0.2008(4) 0.0551(18) Uani 1 1 d . . . . .
H23A H 0.019117 0.251224 0.160521 0.083 Uiso 1 1 calc GR . . . .
H23B H 0.013084 0.102935 0.195640 0.083 Uiso 1 1 calc GR . . . .
H23C H 0.078986 0.151746 0.195409 0.083 Uiso 1 1 calc GR . . . .
C7 C 0.2156(3) 0.4085(7) -0.0063(4) 0.0590(19) Uani 1 1 d . . . . .
H7 H 0.187790 0.336233 -0.033365 0.071 Uiso 1 1 calc R . . . .
B1 B 0.1506(4) 0.5048(8) 0.4294(4) 0.0464(18) Uani 1 1 d . . . . .
C13 C 0.3900(3) 0.8825(7) 0.2346(3) 0.0475(16) Uani 1 1 d . . . . .
H13 H 0.418627 0.919605 0.214804 0.057 Uiso 1 1 calc R . . . .
C20 C 0.4620(3) 0.9216(7) 0.0298(4) 0.0526(18) Uani 1 1 d . . . . .
C27 C 0.0519(3) 0.3221(8) 0.4737(4) 0.062(2) Uani 1 1 d . . . . .
H27A H 0.091804 0.305216 0.517024 0.094 Uiso 1 1 calc GR . . . .
H27B H 0.020951 0.253480 0.474535 0.094 Uiso 1 1 calc GR . . . .
H27C H 0.036973 0.415949 0.477885 0.094 Uiso 1 1 calc GR . . . .
C18 C 0.3877(3) 0.7901(7) 0.0870(4) 0.0521(17) Uani 1 1 d . . . . .
C19 C 0.4219(3) 0.8476(7) 0.0606(4) 0.0559(18) Uani 1 1 d . . . . .
C21 C 0.4988(3) 1.0350(8) 0.0713(4) 0.065(2) Uani 1 1 d . . . . .
H21 H 0.497975 1.059975 0.119638 0.078 Uiso 1 1 calc R . . . .
C15 C 0.3463(3) 0.8779(7) 0.3331(4) 0.0499(16) Uani 1 1 d . . . . .
H15 H 0.344875 0.914544 0.379190 0.060 Uiso 1 1 calc R . . . .
C34 C 0.2993(3) 0.3821(8) 0.4198(5) 0.068(2) Uani 1 1 d . . . . .
C22 C 0.4633(3) 0.8885(8) -0.0423(4) 0.065(2) Uani 1 1 d . . . . .
H22 H 0.438451 0.813984 -0.071653 0.078 Uiso 1 1 calc R . . . .
C9 C 0.2946(3) 0.5816(8) -0.0005(4) 0.0590(19) Uani 1 1 d . . . . .
H9 H 0.319124 0.627876 -0.023536 0.071 Uiso 1 1 calc R . . . .
C8 C 0.2538(4) 0.4789(8) -0.0412(4) 0.065(2) Uani 1 1 d . . . . .
H8 H 0.250434 0.454123 -0.091347 0.078 Uiso 1 1 calc R . . . .
C36 C 0.2671(4) 0.4261(9) 0.5163(4) 0.070(2) Uani 1 1 d . . . . .
C33 C 0.3372(3) 0.3447(10) 0.3729(5) 0.091(3) Uani 1 1 d . . . . .
H33A H 0.318057 0.264484 0.340081 0.136 Uiso 1 1 calc GR . . . .
H33B H 0.380094 0.321432 0.407631 0.136 Uiso 1 1 calc GR . . . .
H33C H 0.337929 0.424094 0.340634 0.136 Uiso 1 1 calc GR . . . .
C32 C 0.1053(4) 0.8003(8) 0.4696(4) 0.070(2) Uani 1 1 d . . . . .
H32A H 0.075490 0.731454 0.473605 0.105 Uiso 1 1 calc GR . . . .
H32B H 0.087524 0.893789 0.466208 0.105 Uiso 1 1 calc GR . . . .
H32C H 0.144486 0.794314 0.515310 0.105 Uiso 1 1 calc GR . . . .
C35 C 0.3183(4) 0.3796(10) 0.5001(5) 0.086(3) Uani 1 1 d . . . . .
H35 H 0.358137 0.351911 0.536651 0.104 Uiso 1 1 calc R . . . .
C37 C 0.2602(4) 0.4398(10) 0.5936(4) 0.092(3) Uani 1 1 d . . . . .
H37A H 0.241355 0.530075 0.595925 0.138 Uiso 1 1 calc GR . . . .
H37B H 0.301522 0.433098 0.635738 0.138 Uiso 1 1 calc GR . . . .
H37C H 0.233238 0.364990 0.598428 0.138 Uiso 1 1 calc GR . . . .
H1 H 0.143(2) 0.533(5) 0.485(3) 0.040(15) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
9 -13 0 0.1032
-9 13 0 0.0884
-16 -1 26 0.1046
16 1 -26 0.1046
-19 6 22 0.1062
30 1 0 0.0166
-30 -1 0 0.0166
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
N3 W1 N1 81.92(15) . . ?
N3 W1 N5 82.17(18) . . ?
C3 W1 N1 90.51(19) . . ?
C3 W1 N3 95.7(2) . . ?
C3 W1 N5 172.35(18) . . ?
N5 W1 N1 81.94(16) . . ?
C1 W1 N1 176.1(2) . . ?
C1 W1 N3 100.55(19) . . ?
C1 W1 C3 86.3(2) . . ?
C1 W1 N5 101.3(2) . . ?
C1 W1 C2 88.4(2) . . ?
C2 W1 N1 89.38(19) . . ?
C2 W1 N3 170.10(19) . . ?
C2 W1 C3 89.1(3) . . ?
C2 W1 N5 92.0(3) . . ?
N2 N1 W1 118.8(3) . . ?
C24 N1 W1 133.4(4) . . ?
C24 N1 N2 107.7(4) . . ?
N4 N3 W1 121.1(3) . . ?
C29 N3 W1 132.5(4) . . ?
C29 N3 N4 106.3(4) . . ?
N1 N2 B1 120.2(4) . . ?
C26 N2 N1 109.1(5) . . ?
C26 N2 B1 130.7(5) . . ?
N3 N4 B1 119.7(5) . . ?
C31 N4 N3 110.3(5) . . ?
C31 N4 B1 129.9(5) . . ?
O2 C3 W1 178.6(5) . . ?
N6 N5 W1 122.2(4) . . ?
C34 N5 W1 131.9(5) . . ?
C34 N5 N6 105.8(6) . . ?
C4 C1 W1 177.7(5) . . ?
N5 N6 B1 118.5(5) . . ?
C36 N6 N5 110.5(6) . . ?
C36 N6 B1 131.0(6) . . ?
O1 C2 W1 178.1(8) . . ?
C17 C4 C1 118.8(5) . . ?
C5 C4 C1 121.2(5) . . ?
C5 C4 C17 120.0(5) . . ?
N2 C26 C25 107.8(5) . . ?
N2 C26 C27 122.9(6) . . ?
C25 C26 C27 129.3(5) . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C29 C28 H28C 109.5 . . ?
N1 C24 C25 108.4(6) . . ?
N1 C24 C23 123.5(5) . . ?
C25 C24 C23 128.1(5) . . ?
C4 C17 C12 120.0(5) . . ?
C16 C17 C4 122.6(5) . . ?
C16 C17 C12 117.3(5) . . ?
C26 C25 C24 107.0(5) . . ?
C26 C25 H25 126.5 . . ?
C24 C25 H25 126.5 . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C7 C6 C5 121.9(6) . . ?
N3 C29 C28 123.0(5) . . ?
N3 C29 C30 109.0(5) . . ?
C30 C29 C28 128.0(5) . . ?
C11 C10 C5 119.5(5) . . ?
C9 C10 C5 119.4(6) . . ?
C9 C10 C11 121.1(5) . . ?
C4 C5 C10 120.1(5) . . ?
C6 C5 C4 122.3(5) . . ?
C6 C5 C10 117.6(5) . . ?
N4 C31 C30 107.1(5) . . ?
N4 C31 C32 123.2(6) . . ?
C30 C31 C32 129.7(6) . . ?
C11 C12 C17 119.6(5) . . ?
C13 C12 C17 118.9(5) . . ?
C13 C12 C11 121.4(5) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 C17 122.0(5) . . ?
C15 C16 H16 119.0 . . ?
C29 C30 H30 126.4 . . ?
C31 C30 C29 107.2(5) . . ?
C31 C30 H30 126.4 . . ?
C13 C14 H14 120.9 . . ?
C13 C14 C15 118.2(6) . . ?
C15 C14 H14 120.9 . . ?
C10 C11 C18 120.4(5) . . ?
C12 C11 C10 120.5(5) . . ?
C12 C11 C18 119.1(5) . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120.0(6) . . ?
C8 C7 H7 120.0 . . ?
N2 B1 H1 112(3) . . ?
N4 B1 N2 108.9(5) . . ?
N4 B1 H1 105(3) . . ?
N6 B1 N2 109.8(5) . . ?
N6 B1 N4 109.8(5) . . ?
N6 B1 H1 111(3) . . ?
C12 C13 H13 118.8 . . ?
C14 C13 C12 122.4(5) . . ?
C14 C13 H13 118.8 . . ?
C21 C20 C19 119.7(6) . . ?
C22 C20 C19 122.1(6) . . ?
C22 C20 C21 118.2(5) . . ?
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 . . ?
C19 C18 C11 178.0(7) . . ?
C18 C19 C20 177.7(8) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.3(6) 3_675 . ?
C22 C21 H21 119.4 3_675 . ?
C16 C15 C14 121.1(6) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
N5 C34 C33 122.7(7) . . ?
N5 C34 C35 109.1(7) . . ?
C35 C34 C33 128.2(7) . . ?
C20 C22 C21 120.6(6) . 3_675 ?
C20 C22 H22 119.7 . . ?
C21 C22 H22 119.7 3_675 . ?
C10 C9 H9 119.1 . . ?
C8 C9 C10 121.8(6) . . ?
C8 C9 H9 119.1 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.2(6) . . ?
C9 C8 H8 120.4 . . ?
N6 C36 C35 107.6(7) . . ?
N6 C36 C37 122.3(8) . . ?
C35 C36 C37 130.0(8) . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C35 C36 107.0(7) . . ?
C34 C35 H35 126.5 . . ?
C36 C35 H35 126.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
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
W1 N1 2.307(4) . ?
W1 N3 2.192(4) . ?
W1 C3 1.997(7) . ?
W1 N5 2.200(5) . ?
W1 C1 1.819(5) . ?
W1 C2 1.990(7) . ?
O2 C3 1.142(7) . ?
N1 N2 1.365(6) . ?
N1 C24 1.337(7) . ?
N3 N4 1.381(6) . ?
N3 C29 1.346(7) . ?
N2 C26 1.349(6) . ?
N2 B1 1.544(9) . ?
N4 C31 1.340(7) . ?
N4 B1 1.542(9) . ?
N5 N6 1.378(7) . ?
N5 C34 1.363(8) . ?
C1 C4 1.444(7) . ?
N6 B1 1.537(9) . ?
N6 C36 1.330(8) . ?
O1 C2 1.139(7) . ?
C4 C17 1.420(8) . ?
C4 C5 1.419(8) . ?
C26 C25 1.364(8) . ?
C26 C27 1.506(8) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28 C29 1.502(8) . ?
C24 C25 1.388(7) . ?
C24 C23 1.499(8) . ?
C17 C12 1.434(7) . ?
C17 C16 1.413(7) . ?
C25 H25 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.402(8) . ?
C6 C7 1.374(9) . ?
C29 C30 1.388(8) . ?
C10 C5 1.432(7) . ?
C10 C11 1.422(8) . ?
C10 C9 1.414(8) . ?
C31 C30 1.377(8) . ?
C31 C32 1.505(8) . ?
C12 C11 1.417(8) . ?
C12 C13 1.402(8) . ?
C16 H16 0.9300 . ?
C16 C15 1.344(8) . ?
C30 H30 0.9300 . ?
C14 H14 0.9300 . ?
C14 C13 1.366(8) . ?
C14 C15 1.419(8) . ?
C11 C18 1.429(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C7 H7 0.9300 . ?
C7 C8 1.430(9) . ?
B1 H1 1.13(5) . ?
C13 H13 0.9300 . ?
C20 C19 1.429(8) . ?
C20 C21 1.389(9) . ?
C20 C22 1.380(8) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C18 C19 1.197(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.380(8) 3_675 ?
C15 H15 0.9300 . ?
C34 C33 1.482(10) . ?
C34 C35 1.374(10) . ?
C22 H22 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.348(9) . ?
C8 H8 0.9300 . ?
C36 C35 1.380(11) . ?
C36 C37 1.501(11) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C35 H35 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
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
W1 N1 N2 C26 -176.0(3) . . . . ?
W1 N1 N2 B1 1.9(6) . . . . ?
W1 N1 C24 C25 175.5(4) . . . . ?
W1 N1 C24 C23 -4.8(8) . . . . ?
W1 N3 N4 C31 -177.8(4) . . . . ?
W1 N3 N4 B1 2.4(7) . . . . ?
W1 N3 C29 C28 -0.4(9) . . . . ?
W1 N3 C29 C30 177.2(4) . . . . ?
W1 N5 N6 B1 0.7(7) . . . . ?
W1 N5 N6 C36 177.6(4) . . . . ?
W1 N5 C34 C33 4.0(11) . . . . ?
W1 N5 C34 C35 -177.6(5) . . . . ?
N1 N2 C26 C25 -0.8(6) . . . . ?
N1 N2 C26 C27 179.1(5) . . . . ?
N1 N2 B1 N4 58.7(7) . . . . ?
N1 N2 B1 N6 -61.5(7) . . . . ?
N1 C24 C25 C26 0.5(7) . . . . ?
N3 N4 C31 C30 -0.1(7) . . . . ?
N3 N4 C31 C32 179.4(6) . . . . ?
N3 N4 B1 N2 -62.7(6) . . . . ?
N3 N4 B1 N6 57.5(7) . . . . ?
N3 C29 C30 C31 1.2(7) . . . . ?
N2 N1 C24 C25 -1.0(6) . . . . ?
N2 N1 C24 C23 178.7(5) . . . . ?
N2 C26 C25 C24 0.2(7) . . . . ?
N4 N3 C29 C28 -178.9(5) . . . . ?
N4 N3 C29 C30 -1.2(6) . . . . ?
N4 C31 C30 C29 -0.7(7) . . . . ?
N5 N6 B1 N2 60.8(7) . . . . ?
N5 N6 B1 N4 -58.9(7) . . . . ?
N5 N6 C36 C35 0.3(8) . . . . ?
N5 N6 C36 C37 -177.9(7) . . . . ?
N5 C34 C35 C36 0.4(9) . . . . ?
C1 C4 C17 C12 176.9(5) . . . . ?
C1 C4 C17 C16 -5.2(8) . . . . ?
C1 C4 C5 C6 1.8(9) . . . . ?
C1 C4 C5 C10 178.9(5) . . . . ?
N6 N5 C34 C33 -178.6(7) . . . . ?
N6 N5 C34 C35 -0.2(8) . . . . ?
N6 C36 C35 C34 -0.4(9) . . . . ?
C4 C17 C12 C11 3.9(9) . . . . ?
C4 C17 C12 C13 179.4(5) . . . . ?
C4 C17 C16 C15 -177.5(6) . . . . ?
C26 N2 B1 N4 -123.9(6) . . . . ?
C26 N2 B1 N6 115.9(6) . . . . ?
C28 C29 C30 C31 178.7(6) . . . . ?
C24 N1 N2 C26 1.1(6) . . . . ?
C24 N1 N2 B1 179.0(5) . . . . ?
C17 C4 C5 C6 -177.8(6) . . . . ?
C17 C4 C5 C10 -0.7(9) . . . . ?
C17 C12 C11 C10 0.1(9) . . . . ?
C17 C12 C11 C18 178.6(6) . . . . ?
C17 C12 C13 C14 -2.4(10) . . . . ?
C17 C16 C15 C14 -1.2(10) . . . . ?
C6 C7 C8 C9 1.2(12) . . . . ?
C29 N3 N4 C31 0.8(6) . . . . ?
C29 N3 N4 B1 -179.0(5) . . . . ?
C10 C9 C8 C7 0.6(12) . . . . ?
C5 C4 C17 C12 -3.6(8) . . . . ?
C5 C4 C17 C16 174.3(5) . . . . ?
C5 C6 C7 C8 -1.5(11) . . . . ?
C5 C10 C11 C12 -4.3(9) . . . . ?
C5 C10 C11 C18 177.2(6) . . . . ?
C5 C10 C9 C8 -2.1(11) . . . . ?
C31 N4 B1 N2 117.6(7) . . . . ?
C31 N4 B1 N6 -122.3(7) . . . . ?
C12 C17 C16 C15 0.4(9) . . . . ?
C16 C17 C12 C11 -174.1(5) . . . . ?
C16 C17 C12 C13 1.4(8) . . . . ?
C11 C10 C5 C4 4.7(9) . . . . ?
C11 C10 C5 C6 -178.1(6) . . . . ?
C11 C10 C9 C8 177.8(7) . . . . ?
C11 C12 C13 C14 173.0(6) . . . . ?
C23 C24 C25 C26 -179.1(6) . . . . ?
C7 C6 C5 C4 177.1(6) . . . . ?
C7 C6 C5 C10 -0.1(10) . . . . ?
B1 N2 C26 C25 -178.4(6) . . . . ?
B1 N2 C26 C27 1.5(10) . . . . ?
B1 N4 C31 C30 179.7(6) . . . . ?
B1 N4 C31 C32 -0.8(11) . . . . ?
B1 N6 C36 C35 176.7(7) . . . . ?
B1 N6 C36 C37 -1.5(11) . . . . ?
C13 C12 C11 C10 -175.3(6) . . . . ?
C13 C12 C11 C18 3.2(9) . . . . ?
C13 C14 C15 C16 0.2(10) . . . . ?
C27 C26 C25 C24 -179.8(6) . . . . ?
C19 C20 C21 C22 -178.1(7) . . . 3_675 ?
C19 C20 C22 C21 178.0(7) . . . 3_675 ?
C21 C20 C22 C21 1.1(13) . . . 3_675 ?
C15 C14 C13 C12 1.6(10) . . . . ?
C34 N5 N6 B1 -177.0(6) . . . . ?
C34 N5 N6 C36 -0.1(7) . . . . ?
C22 C20 C21 C22 -1.1(14) . . . 3_675 ?
C9 C10 C5 C4 -175.4(6) . . . . ?
C9 C10 C5 C6 1.8(9) . . . . ?
C9 C10 C11 C12 175.7(6) . . . . ?
C9 C10 C11 C18 -2.8(10) . . . . ?
C36 N6 B1 N2 -115.4(7) . . . . ?
C36 N6 B1 N4 125.0(7) . . . . ?
C33 C34 C35 C36 178.7(8) . . . . ?
C32 C31 C30 C29 179.9(7) . . . . ?
C37 C36 C35 C34 177.6(8) . . . . ?
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
9.0908 -12.6224 0.0682 -0.1991 -0.8276 0.5249
-9.0235 12.6246 -0.1734 0.1986 0.8255 -0.5284
-16.0207 -1.1620 25.7385 0.1103 0.4704 0.8755
16.0207 1.1620 -25.7385 -0.1103 -0.4704 -0.8755
-18.7674 6.4462 21.5261 0.2094 0.8806 0.4251
29.6607 0.5979 -0.4372 0.8531 -0.5216 0.0091
-29.6607 -0.5979 0.4372 -0.8531 0.5216 -0.0091
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 -0.143 -0.717 574.6 104.2 ?
