#------------------------------------------------------------------------------
#$Date: 2022-02-04 21:40:18 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272672 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/91/7709144.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_7709144
loop_
_publ_author_name
'Frogley, Benjamin J.'
'Hill, Anthony F.'
_publ_section_title
;
 Arsinocarbyne reactivity.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1907
_journal_page_last               1917
_journal_paper_doi               10.1039/d1dt03790k
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C40 H46 As B Cl2 N6 O2 Os W'
_chemical_formula_sum            'C40 H46 As B Cl2 N6 O2 Os W'
_chemical_formula_weight         1173.51
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-22 deposited with the CCDC.	2021-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.454(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4992(5)
_cell_length_b                   12.8152(2)
_cell_length_c                   18.7410(4)
_cell_measurement_reflns_used    10634
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.5670
_cell_measurement_theta_min      4.3700
_cell_volume                     4155.71(19)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -102.00 -19.00   1.00    7.00    --  -36.03 -38.00-120.00   83
  2  ω    -78.00  31.00   1.00    7.00    --  -36.03   0.00  90.00  109
  3  ω    -51.00  20.00   1.00    7.00    --  -36.03  57.00 120.00   71
  4  ω      7.00  73.00   1.00    7.00    --   36.03 -99.00-150.00   66
  5  ω     33.00  96.00   1.00    7.00    --   36.03-136.00  54.00   63
  6  ω    117.00 159.00   1.00   30.00    --  105.15  61.00  30.00   42
  7  ω     38.00 114.00   1.00   30.00    --  105.15 -45.00-180.00   76
  8  ω     44.00 164.00   1.00   30.00    --  105.15   0.00  30.00  120
  9  ω     38.00 115.00   1.00   30.00    --  105.15 -45.00 -30.00   77
 10  ω     60.00 109.00   1.00   30.00    --  105.15-111.00 -30.00   49
 11  ω     58.00 123.00   1.00   30.00    --  105.15 -45.00-120.00   65
 12  ω     53.00 105.00   1.00   30.00    --  105.15 -95.00-150.00   52
 13  ω     37.00 123.00   1.00   30.00    --  105.15 -45.00  90.00   86
 14  ω     50.00 106.00   1.00   30.00    --  105.15 -95.00 120.00   56
 15  ω    103.00 173.00   1.00   30.00    --  105.15  77.00-120.00   70
 16  ω     53.00 124.00   1.00   30.00    --  105.15 -77.00 -30.00   71
;
_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      -0.0068656000
_diffrn_orient_matrix_UB_12      0.0947136000
_diffrn_orient_matrix_UB_13      -0.0534826000
_diffrn_orient_matrix_UB_21      -0.0887467000
_diffrn_orient_matrix_UB_22      -0.0078359000
_diffrn_orient_matrix_UB_23      -0.0392485000
_diffrn_orient_matrix_UB_31      -0.0007505000
_diffrn_orient_matrix_UB_32      0.0736166000
_diffrn_orient_matrix_UB_33      0.0646777000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22135
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.812
_diffrn_reflns_theta_min         4.293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40479
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.976
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0327
_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)+(0.0480P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6820
_reflns_number_total             7880
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03790k2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7709141--7709146.cif.'
_cod_original_cell_volume        4155.71(18)
_cod_database_code               7709144
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H46 As B Cl2 N6 O2 Os W'
_chemical_oxdiff_usercomment     'CDCl3 sit'
_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 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C38(H38), B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C34(H34), C36(H36), C5(H5), C37(H37), C9(H9), C8(H8), C28(H28),
 C7(H7), C18(H18), C15(H15), C23(H23), C6(H6), C11(H11), C12(H12), C14(H14),
 C13(H13)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C16(H16A,H16B,H16C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C)
;
_ins_header
;
TITL BF163A_scale05filt in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  19.499216  12.815164  18.741048  90.0000 117.4542  90.0000
ZERR    4.00   0.000456   0.000176   0.000449   0.0000   0.0030   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Cl As W Os
UNIT 160.00 184.00 4.00 24.00 8.00 8.00 4.00 4.00 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 2.121
_oxdiff_exptl_absorpt_empirical_full_min 0.674
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
Os1 Os 0.35370(2) 0.06309(2) 0.47849(2) 0.02515(7) Uani 1 1 d . . . . .
W1 W 0.18586(2) 0.29925(2) 0.56655(2) 0.02514(7) Uani 1 1 d . . . . .
As1 As 0.26136(3) 0.04418(4) 0.53396(3) 0.02305(11) Uani 1 1 d . . . . .
Cl1 Cl 0.44850(7) 0.08008(11) 0.61748(7) 0.0340(3) Uani 1 1 d . . . . .
Cl2 Cl 0.36687(8) -0.12559(10) 0.49417(8) 0.0365(3) Uani 1 1 d . . . . .
N5 N 0.1733(2) 0.3898(3) 0.4607(3) 0.0276(8) Uani 1 1 d . . . . .
N6 N 0.1974(3) 0.4915(3) 0.4694(3) 0.0314(9) Uani 1 1 d . . . . .
N3 N 0.2952(2) 0.3829(4) 0.6321(3) 0.0325(9) Uani 1 1 d . . . . .
N4 N 0.3047(2) 0.4829(3) 0.6106(3) 0.0316(9) Uani 1 1 d . . . . .
O1 O 0.1821(3) 0.2085(3) 0.7205(3) 0.0483(11) Uani 1 1 d . . . . .
O2 O 0.0188(2) 0.2055(4) 0.4712(3) 0.0545(13) Uani 1 1 d . . . . .
N1 N 0.1375(3) 0.4544(3) 0.5886(3) 0.0316(9) Uani 1 1 d . . . . .
N2 N 0.1723(3) 0.5450(3) 0.5830(3) 0.0298(9) Uani 1 1 d . . . . .
C33 C 0.4024(4) 0.0663(5) 0.3931(4) 0.0436(14) Uani 1 1 d . . . . .
H33 H 0.438478 0.022330 0.389175 0.052 Uiso 1 1 calc R U . . .
C4 C 0.2903(3) -0.0282(4) 0.6360(3) 0.0271(10) Uani 1 1 d . . . . .
C34 C 0.4280(3) 0.1542(5) 0.4416(3) 0.0360(12) Uani 1 1 d . . . . .
H34 H 0.480823 0.167550 0.469097 0.043 Uiso 1 1 calc R U . . .
C10 C 0.1642(3) -0.0236(4) 0.4608(3) 0.0285(10) Uani 1 1 d . . . . .
C36 C 0.2951(3) 0.2001(4) 0.4080(3) 0.0294(10) Uani 1 1 d . . . . .
H36 H 0.259216 0.242834 0.413417 0.035 Uiso 1 1 calc R U . . .
C5 C 0.2481(4) -0.0077(4) 0.6771(3) 0.0383(12) Uani 1 1 d . . . . .
H5 H 0.206657 0.038466 0.655359 0.046 Uiso 1 1 calc R U . . .
C19 C 0.1399(3) 0.6273(4) 0.6013(3) 0.0347(11) Uani 1 1 d . . . . .
C29 C 0.1756(4) 0.5350(5) 0.3970(4) 0.0406(13) Uani 1 1 d . . . . .
C26 C 0.1010(3) 0.2657(4) 0.3485(3) 0.0352(11) Uani 1 1 d . . . . .
H26A H 0.129049 0.211969 0.386491 0.053 Uiso 1 1 calc R U . . .
H26B H 0.103062 0.253077 0.298983 0.053 Uiso 1 1 calc R U . . .
H26C H 0.048143 0.265409 0.338632 0.053 Uiso 1 1 calc R U . . .
C37 C 0.2686(3) 0.1106(4) 0.3573(3) 0.0333(11) Uani 1 1 d . . . . .
H37 H 0.215815 0.097338 0.329384 0.040 Uiso 1 1 calc R U . . .
C24 C 0.3792(4) 0.5137(5) 0.6556(4) 0.0434(14) Uani 1 1 d . . . . .
C35 C 0.3750(3) 0.2259(4) 0.4506(3) 0.0327(11) Uani 1 1 d . . . . .
C2 C 0.1857(3) 0.2417(4) 0.6659(3) 0.0344(11) Uani 1 1 d . . . . .
C17 C 0.0838(3) 0.4794(4) 0.6105(4) 0.0361(12) Uani 1 1 d . . . . .
C3 C 0.0786(3) 0.2418(4) 0.5055(4) 0.0369(12) Uani 1 1 d . . . . .
C21 C 0.3775(3) 0.2493(5) 0.7316(4) 0.0448(14) Uani 1 1 d . . . . .
H21A H 0.335913 0.234444 0.743985 0.067 Uiso 1 1 calc R U . . .
H21B H 0.425467 0.250339 0.780418 0.067 Uiso 1 1 calc R U . . .
H21C H 0.379585 0.196444 0.696405 0.067 Uiso 1 1 calc R U . . .
C9 C 0.3510(3) -0.0977(4) 0.6677(3) 0.0340(11) Uani 1 1 d . . . . .
H9 H 0.379488 -0.111621 0.640355 0.041 Uiso 1 1 calc R U . . .
C1 C 0.2220(3) 0.1744(4) 0.5511(3) 0.0272(10) Uani 1 1 d . . . . .
C8 C 0.3698(4) -0.1469(5) 0.7405(4) 0.0423(13) Uani 1 1 d . . . . .
H8 H 0.410232 -0.194757 0.761339 0.051 Uiso 1 1 calc R U . . .
C28 C 0.1372(4) 0.4589(5) 0.3393(4) 0.0407(13) Uani 1 1 d . . . . .
H28 H 0.116208 0.466076 0.283798 0.049 Uiso 1 1 calc R U . . .
C7 C 0.3288(4) -0.1249(5) 0.7817(3) 0.0441(14) Uani 1 1 d . . . . .
H7 H 0.342343 -0.156970 0.830936 0.053 Uiso 1 1 calc R U . . .
C18 C 0.0835(3) 0.5876(5) 0.6194(4) 0.0398(12) Uani 1 1 d . . . . .
H18 H 0.051686 0.625674 0.634511 0.048 Uiso 1 1 calc R U . . .
C32 C 0.3208(3) 0.0413(5) 0.3483(3) 0.0362(12) Uani 1 1 d . . . . .
C15 C 0.1589(4) -0.0794(5) 0.3957(4) 0.0395(13) Uani 1 1 d . . . . .
H15 H 0.202345 -0.087302 0.387721 0.047 Uiso 1 1 calc R U . . .
C23 C 0.4173(3) 0.4321(5) 0.7073(4) 0.0462(15) Uani 1 1 d . . . . .
H23 H 0.469023 0.431236 0.745623 0.055 Uiso 1 1 calc R U . . .
C22 C 0.3646(3) 0.3524(5) 0.6917(3) 0.0367(12) Uani 1 1 d . . . . .
C6 C 0.2671(4) -0.0555(5) 0.7507(4) 0.0466(15) Uani 1 1 d . . . . .
H6 H 0.239146 -0.041116 0.778461 0.056 Uiso 1 1 calc R U . . .
C11 C 0.1001(4) -0.0148(5) 0.4733(4) 0.0436(13) Uani 1 1 d . . . . .
H11 H 0.103647 0.020919 0.518083 0.052 Uiso 1 1 calc R U . . .
C27 C 0.1366(3) 0.3697(4) 0.3817(3) 0.0318(11) Uani 1 1 d . . . . .
C20 C 0.1638(4) 0.7375(5) 0.5999(5) 0.0489(16) Uani 1 1 d . . . . .
H20A H 0.218116 0.744615 0.635121 0.073 Uiso 1 1 calc R U . . .
H20B H 0.135473 0.782866 0.617632 0.073 Uiso 1 1 calc R U . . .
H20C H 0.153148 0.755903 0.546167 0.073 Uiso 1 1 calc R U . . .
C25 C 0.4092(4) 0.6164(6) 0.6460(5) 0.0574(18) Uani 1 1 d . . . . .
H25A H 0.411741 0.617666 0.596032 0.086 Uiso 1 1 calc R U . . .
H25B H 0.459912 0.627249 0.689681 0.086 Uiso 1 1 calc R U . . .
H25C H 0.375293 0.670725 0.645991 0.086 Uiso 1 1 calc R U . . .
C31 C 0.2951(5) -0.0539(5) 0.2987(4) 0.0557(18) Uani 1 1 d . . . . .
H31A H 0.327916 -0.111232 0.327527 0.084 Uiso 1 1 calc R U . . .
H31B H 0.298025 -0.043092 0.249436 0.084 Uiso 1 1 calc R U . . .
H31C H 0.242772 -0.069421 0.286733 0.084 Uiso 1 1 calc R U . . .
C12 C 0.0299(4) -0.0593(6) 0.4191(5) 0.0555(18) Uani 1 1 d . . . . .
H12 H -0.013529 -0.051504 0.427091 0.067 Uiso 1 1 calc R U . . .
C30 C 0.1933(6) 0.6458(5) 0.3861(4) 0.063(2) Uani 1 1 d . . . . .
H30A H 0.175426 0.691261 0.414672 0.094 Uiso 1 1 calc R U . . .
H30B H 0.167780 0.663081 0.329912 0.094 Uiso 1 1 calc R U . . .
H30C H 0.248113 0.653950 0.406617 0.094 Uiso 1 1 calc R U . . .
C14 C 0.0895(4) -0.1235(5) 0.3420(4) 0.0512(16) Uani 1 1 d . . . . .
H14 H 0.086236 -0.159681 0.297512 0.061 Uiso 1 1 calc R U . . .
C16 C 0.0320(4) 0.4015(5) 0.6209(4) 0.0477(15) Uani 1 1 d . . . . .
H16A H -0.002008 0.371493 0.569725 0.072 Uiso 1 1 calc R U . . .
H16B H 0.001971 0.435616 0.642775 0.072 Uiso 1 1 calc R U . . .
H16C H 0.062691 0.347490 0.656970 0.072 Uiso 1 1 calc R U . . .
C38 C 0.3975(4) 0.3248(5) 0.5017(4) 0.0468(14) Uani 1 1 d . . . . .
H38 H 0.372236 0.324433 0.536304 0.056 Uiso 1 1 calc R U . . .
C13 C 0.0248(4) -0.1144(5) 0.3540(4) 0.0512(16) Uani 1 1 d . . . . .
H13 H -0.021587 -0.145392 0.318396 0.061 Uiso 1 1 calc R U . . .
C39 C 0.3688(5) 0.4182(6) 0.4456(5) 0.0586(18) Uani 1 1 d . . . . .
H39A H 0.393842 0.419739 0.411917 0.088 Uiso 1 1 calc R U . . .
H39B H 0.380438 0.481183 0.476753 0.088 Uiso 1 1 calc R U . . .
H39C H 0.313916 0.412740 0.412677 0.088 Uiso 1 1 calc R U . . .
B1 B 0.2339(3) 0.5457(4) 0.5529(4) 0.0301(12) Uani 1 1 d . . . . .
H1 H 0.248738 0.617502 0.548303 0.036 Uiso 1 1 calc R U . . .
C40 C 0.4844(5) 0.3321(7) 0.5541(5) 0.064(2) Uani 1 1 d . . . . .
H40A H 0.502589 0.270137 0.586218 0.096 Uiso 1 1 calc R U . . .
H40B H 0.496217 0.391910 0.588539 0.096 Uiso 1 1 calc R U . . .
H40C H 0.509414 0.338745 0.520525 0.096 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 '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
10 -1 1 0.0055
-10 1 -1 0.0055
-5 5 10 0.0405
5 -5 -10 0.0405
5 -3 -11 0.0425
-5 3 11 0.0425
2 7 -5 0.0657
-2 -7 5 0.0657
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
Cl1 Os1 As1 84.19(3) . . ?
Cl1 Os1 Cl2 88.49(5) . . ?
Cl2 Os1 As1 84.75(3) . . ?
C33 Os1 As1 161.43(18) . . ?
C33 Os1 Cl1 114.21(17) . . ?
C33 Os1 Cl2 92.84(18) . . ?
C33 Os1 C34 36.6(2) . . ?
C33 Os1 C35 68.0(2) . . ?
C33 Os1 C32 38.2(2) . . ?
C34 Os1 As1 153.54(17) . . ?
C34 Os1 Cl1 90.22(14) . . ?
C34 Os1 Cl2 121.02(16) . . ?
C34 Os1 C35 38.1(2) . . ?
C34 Os1 C32 67.9(2) . . ?
C36 Os1 As1 93.09(14) . . ?
C36 Os1 Cl1 120.60(14) . . ?
C36 Os1 Cl2 150.54(14) . . ?
C36 Os1 C33 80.0(2) . . ?
C36 Os1 C34 67.7(2) . . ?
C36 Os1 C37 38.1(2) . . ?
C36 Os1 C35 37.6(2) . . ?
C36 Os1 C32 68.4(2) . . ?
C37 Os1 As1 96.48(15) . . ?
C37 Os1 Cl1 158.67(16) . . ?
C37 Os1 Cl2 112.82(16) . . ?
C37 Os1 C33 67.5(2) . . ?
C37 Os1 C34 79.7(2) . . ?
C37 Os1 C35 68.4(2) . . ?
C37 Os1 C32 37.3(2) . . ?
C35 Os1 As1 116.06(15) . . ?
C35 Os1 Cl1 92.06(14) . . ?
C35 Os1 Cl2 159.14(15) . . ?
C32 Os1 As1 123.28(16) . . ?
C32 Os1 Cl1 151.86(16) . . ?
C32 Os1 Cl2 88.22(16) . . ?
C32 Os1 C35 81.5(2) . . ?
N5 W1 N1 79.86(16) . . ?
N3 W1 N5 85.57(17) . . ?
N3 W1 N1 81.42(17) . . ?
C2 W1 N5 168.31(19) . . ?
C2 W1 N3 94.4(2) . . ?
C2 W1 N1 88.58(19) . . ?
C3 W1 N5 91.5(2) . . ?
C3 W1 N3 172.1(2) . . ?
C3 W1 N1 90.8(2) . . ?
C3 W1 C2 87.0(2) . . ?
C1 W1 N5 102.06(18) . . ?
C1 W1 N3 99.84(19) . . ?
C1 W1 N1 177.76(19) . . ?
C1 W1 C2 89.5(2) . . ?
C1 W1 C3 88.0(2) . . ?
C4 As1 Os1 121.26(15) . . ?
C10 As1 Os1 114.00(16) . . ?
C10 As1 C4 102.9(2) . . ?
C1 As1 Os1 114.15(14) . . ?
C1 As1 C4 101.8(2) . . ?
C1 As1 C10 99.8(2) . . ?
N6 N5 W1 120.2(3) . . ?
C27 N5 W1 132.2(4) . . ?
C27 N5 N6 107.1(4) . . ?
N5 N6 B1 121.2(4) . . ?
C29 N6 N5 110.1(5) . . ?
C29 N6 B1 128.1(5) . . ?
N4 N3 W1 121.1(3) . . ?
C22 N3 W1 131.7(4) . . ?
C22 N3 N4 107.0(5) . . ?
N3 N4 B1 119.7(4) . . ?
C24 N4 N3 109.7(5) . . ?
C24 N4 B1 130.0(5) . . ?
N2 N1 W1 117.1(3) . . ?
C17 N1 W1 134.8(4) . . ?
C17 N1 N2 108.0(4) . . ?
N1 N2 B1 121.9(4) . . ?
C19 N2 N1 109.5(5) . . ?
C19 N2 B1 128.4(5) . . ?
Os1 C33 H33 129.8 . . ?
C34 C33 Os1 71.7(3) . . ?
C34 C33 H33 119.1 . . ?
C34 C33 C32 121.7(5) . . ?
C32 C33 Os1 72.0(3) . . ?
C32 C33 H33 119.1 . . ?
C5 C4 As1 118.3(4) . . ?
C9 C4 As1 122.0(4) . . ?
C9 C4 C5 119.7(5) . . ?
Os1 C34 H34 130.0 . . ?
C33 C34 Os1 71.7(3) . . ?
C33 C34 H34 119.0 . . ?
C33 C34 C35 122.0(5) . . ?
C35 C34 Os1 72.0(3) . . ?
C35 C34 H34 119.0 . . ?
C15 C10 As1 120.3(4) . . ?
C15 C10 C11 119.3(5) . . ?
C11 C10 As1 120.4(4) . . ?
Os1 C36 H36 128.3 . . ?
C37 C36 Os1 71.5(3) . . ?
C37 C36 H36 119.1 . . ?
C35 C36 Os1 73.4(3) . . ?
C35 C36 H36 119.1 . . ?
C35 C36 C37 121.8(5) . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.7(5) . . ?
C6 C5 H5 119.7 . . ?
N2 C19 C18 107.0(5) . . ?
N2 C19 C20 123.2(5) . . ?
C18 C19 C20 129.9(5) . . ?
N6 C29 C28 107.5(5) . . ?
N6 C29 C30 123.1(6) . . ?
C28 C29 C30 129.3(6) . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C27 C26 H26C 109.5 . . ?
Os1 C37 H37 130.1 . . ?
C36 C37 Os1 70.4(3) . . ?
C36 C37 H37 119.2 . . ?
C32 C37 Os1 73.0(3) . . ?
C32 C37 C36 121.5(5) . . ?
C32 C37 H37 119.2 . . ?
N4 C24 C23 106.8(6) . . ?
N4 C24 C25 123.4(6) . . ?
C23 C24 C25 129.8(6) . . ?
C34 C35 Os1 69.8(3) . . ?
C34 C35 C38 125.7(5) . . ?
C36 C35 Os1 69.0(3) . . ?
C36 C35 C34 116.2(5) . . ?
C36 C35 C38 118.0(5) . . ?
C38 C35 Os1 131.3(4) . . ?
O1 C2 W1 177.0(5) . . ?
N1 C17 C18 108.8(5) . . ?
N1 C17 C16 123.8(5) . . ?
C18 C17 C16 127.4(5) . . ?
O2 C3 W1 177.5(5) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
C4 C9 H9 119.9 . . ?
C4 C9 C8 120.1(6) . . ?
C8 C9 H9 119.9 . . ?
W1 C1 As1 178.8(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 C9 120.0(6) . . ?
C7 C8 H8 120.0 . . ?
C29 C28 H28 127.0 . . ?
C29 C28 C27 105.9(5) . . ?
C27 C28 H28 127.0 . . ?
C8 C7 H7 119.6 . . ?
C8 C7 C6 120.8(5) . . ?
C6 C7 H7 119.6 . . ?
C19 C18 C17 106.7(5) . . ?
C19 C18 H18 126.6 . . ?
C17 C18 H18 126.6 . . ?
C33 C32 Os1 69.8(3) . . ?
C33 C32 C31 120.7(6) . . ?
C37 C32 Os1 69.7(3) . . ?
C37 C32 C33 116.7(5) . . ?
C37 C32 C31 122.6(6) . . ?
C31 C32 Os1 129.4(4) . . ?
C10 C15 H15 119.8 . . ?
C10 C15 C14 120.4(6) . . ?
C14 C15 H15 119.8 . . ?
C24 C23 H23 126.2 . . ?
C22 C23 C24 107.7(5) . . ?
C22 C23 H23 126.2 . . ?
N3 C22 C21 123.1(5) . . ?
N3 C22 C23 108.8(6) . . ?
C23 C22 C21 128.0(5) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 C5 118.7(6) . . ?
C7 C6 H6 120.6 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.4(6) . . ?
C12 C11 H11 119.8 . . ?
N5 C27 C26 122.6(5) . . ?
N5 C27 C28 109.4(5) . . ?
C28 C27 C26 128.0(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.1(7) . . ?
C13 C12 H12 120.0 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C15 C14 H14 119.8 . . ?
C15 C14 C13 120.5(6) . . ?
C13 C14 H14 119.8 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C35 C38 H38 108.9 . . ?
C39 C38 C35 108.2(5) . . ?
C39 C38 H38 108.9 . . ?
C39 C38 C40 110.1(6) . . ?
C40 C38 C35 111.7(6) . . ?
C40 C38 H38 108.9 . . ?
C12 C13 C14 119.3(6) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
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 . . ?
N6 B1 H1 110.4 . . ?
N4 B1 N6 108.8(4) . . ?
N4 B1 N2 109.7(5) . . ?
N4 B1 H1 110.4 . . ?
N2 B1 N6 107.0(4) . . ?
N2 B1 H1 110.4 . . ?
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 . . ?
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
Os1 As1 2.4715(5) . ?
Os1 Cl1 2.4103(12) . ?
Os1 Cl2 2.4351(13) . ?
Os1 C33 2.206(6) . ?
Os1 C34 2.206(5) . ?
Os1 C36 2.178(5) . ?
Os1 C37 2.193(5) . ?
Os1 C35 2.236(5) . ?
Os1 C32 2.236(5) . ?
W1 N5 2.212(4) . ?
W1 N3 2.189(4) . ?
W1 N1 2.318(4) . ?
W1 C2 2.005(5) . ?
W1 C3 2.005(5) . ?
W1 C1 1.824(5) . ?
As1 C4 1.960(5) . ?
As1 C10 1.956(5) . ?
As1 C1 1.925(5) . ?
N5 N6 1.369(6) . ?
N5 C27 1.340(7) . ?
N6 C29 1.342(8) . ?
N6 B1 1.553(7) . ?
N3 N4 1.381(7) . ?
N3 C22 1.356(7) . ?
N4 C24 1.360(7) . ?
N4 B1 1.532(7) . ?
O1 C2 1.138(7) . ?
O2 C3 1.140(7) . ?
N1 N2 1.372(6) . ?
N1 C17 1.329(7) . ?
N2 C19 1.354(7) . ?
N2 B1 1.544(8) . ?
C33 H33 0.9300 . ?
C33 C34 1.387(9) . ?
C33 C32 1.452(9) . ?
C4 C5 1.388(8) . ?
C4 C9 1.378(7) . ?
C34 H34 0.9300 . ?
C34 C35 1.452(8) . ?
C10 C15 1.378(8) . ?
C10 C11 1.379(8) . ?
C36 H36 0.9300 . ?
C36 C37 1.427(8) . ?
C36 C35 1.423(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.393(8) . ?
C19 C18 1.387(9) . ?
C19 C20 1.491(8) . ?
C29 C28 1.390(9) . ?
C29 C30 1.497(8) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C26 C27 1.499(7) . ?
C37 H37 0.9300 . ?
C37 C32 1.418(8) . ?
C24 C23 1.386(10) . ?
C24 C25 1.484(10) . ?
C35 C38 1.525(9) . ?
C17 C18 1.397(8) . ?
C17 C16 1.495(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 C22 1.481(9) . ?
C9 H9 0.9300 . ?
C9 C8 1.391(8) . ?
C8 H8 0.9300 . ?
C8 C7 1.373(9) . ?
C28 H28 0.9300 . ?
C28 C27 1.395(8) . ?
C7 H7 0.9300 . ?
C7 C6 1.390(9) . ?
C18 H18 0.9300 . ?
C32 C31 1.475(9) . ?
C15 H15 0.9300 . ?
C15 C14 1.382(8) . ?
C23 H23 0.9300 . ?
C23 C22 1.382(9) . ?
C6 H6 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.396(9) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C12 H12 0.9300 . ?
C12 C13 1.374(11) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C14 H14 0.9300 . ?
C14 C13 1.385(10) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C38 H38 0.9800 . ?
C38 C39 1.519(9) . ?
C38 C40 1.520(10) . ?
C13 H13 0.9300 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
B1 H1 0.9800 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 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
Os1 C33 C34 C35 -53.8(5) . . . . ?
Os1 C33 C32 C37 53.3(4) . . . . ?
Os1 C33 C32 C31 -124.6(5) . . . . ?
Os1 C34 C35 C36 -52.6(4) . . . . ?
Os1 C34 C35 C38 127.0(5) . . . . ?
Os1 C36 C37 C32 -54.3(5) . . . . ?
Os1 C36 C35 C34 53.1(4) . . . . ?
Os1 C36 C35 C38 -126.6(5) . . . . ?
Os1 C37 C32 C33 -53.3(4) . . . . ?
Os1 C37 C32 C31 124.5(6) . . . . ?
Os1 C35 C38 C39 -154.0(5) . . . . ?
Os1 C35 C38 C40 84.6(7) . . . . ?
W1 N5 N6 C29 -172.2(4) . . . . ?
W1 N5 N6 B1 0.1(6) . . . . ?
W1 N5 C27 C26 -7.8(8) . . . . ?
W1 N5 C27 C28 171.6(4) . . . . ?
W1 N3 N4 C24 -174.6(4) . . . . ?
W1 N3 N4 B1 13.4(6) . . . . ?
W1 N3 C22 C21 -6.2(8) . . . . ?
W1 N3 C22 C23 174.4(4) . . . . ?
W1 N1 N2 C19 -177.0(3) . . . . ?
W1 N1 N2 B1 7.6(6) . . . . ?
W1 N1 C17 C18 176.0(4) . . . . ?
W1 N1 C17 C16 -5.6(9) . . . . ?
As1 C4 C5 C6 -178.8(5) . . . . ?
As1 C4 C9 C8 179.7(4) . . . . ?
As1 C10 C15 C14 -177.2(5) . . . . ?
As1 C10 C11 C12 177.1(5) . . . . ?
N5 N6 C29 C28 -0.9(7) . . . . ?
N5 N6 C29 C30 -179.9(6) . . . . ?
N5 N6 B1 N4 57.4(6) . . . . ?
N5 N6 B1 N2 -61.1(6) . . . . ?
N6 N5 C27 C26 -179.2(5) . . . . ?
N6 N5 C27 C28 0.2(6) . . . . ?
N6 C29 C28 C27 1.0(7) . . . . ?
N3 N4 C24 C23 -0.9(7) . . . . ?
N3 N4 C24 C25 178.3(6) . . . . ?
N3 N4 B1 N6 -65.4(6) . . . . ?
N3 N4 B1 N2 51.3(6) . . . . ?
N4 N3 C22 C21 179.1(5) . . . . ?
N4 N3 C22 C23 -0.3(6) . . . . ?
N4 C24 C23 C22 0.7(7) . . . . ?
N1 N2 C19 C18 0.3(6) . . . . ?
N1 N2 C19 C20 -179.2(5) . . . . ?
N1 N2 B1 N6 54.7(6) . . . . ?
N1 N2 B1 N4 -63.2(6) . . . . ?
N1 C17 C18 C19 0.3(7) . . . . ?
N2 N1 C17 C18 -0.1(6) . . . . ?
N2 N1 C17 C16 178.4(6) . . . . ?
N2 C19 C18 C17 -0.4(7) . . . . ?
C33 C34 C35 Os1 53.7(5) . . . . ?
C33 C34 C35 C36 1.1(8) . . . . ?
C33 C34 C35 C38 -179.3(5) . . . . ?
C4 C5 C6 C7 -0.7(10) . . . . ?
C4 C9 C8 C7 -1.2(9) . . . . ?
C34 C33 C32 Os1 -53.9(5) . . . . ?
C34 C33 C32 C37 -0.6(8) . . . . ?
C34 C33 C32 C31 -178.6(6) . . . . ?
C34 C35 C38 C39 112.2(7) . . . . ?
C34 C35 C38 C40 -9.2(8) . . . . ?
C10 C15 C14 C13 -1.5(11) . . . . ?
C10 C11 C12 C13 1.7(11) . . . . ?
C36 C37 C32 Os1 53.1(4) . . . . ?
C36 C37 C32 C33 -0.2(8) . . . . ?
C36 C37 C32 C31 177.6(5) . . . . ?
C36 C35 C38 C39 -68.2(7) . . . . ?
C36 C35 C38 C40 170.4(5) . . . . ?
C5 C4 C9 C8 0.0(8) . . . . ?
C19 N2 B1 N6 -119.8(5) . . . . ?
C19 N2 B1 N4 122.4(5) . . . . ?
C29 N6 B1 N4 -131.7(6) . . . . ?
C29 N6 B1 N2 109.8(6) . . . . ?
C29 C28 C27 N5 -0.7(7) . . . . ?
C29 C28 C27 C26 178.6(6) . . . . ?
C37 C36 C35 Os1 -55.0(4) . . . . ?
C37 C36 C35 C34 -1.9(7) . . . . ?
C37 C36 C35 C38 178.4(5) . . . . ?
C24 N4 B1 N6 124.4(6) . . . . ?
C24 N4 B1 N2 -118.8(6) . . . . ?
C24 C23 C22 N3 -0.2(7) . . . . ?
C24 C23 C22 C21 -179.6(6) . . . . ?
C35 C36 C37 Os1 55.9(4) . . . . ?
C35 C36 C37 C32 1.6(8) . . . . ?
C17 N1 N2 C19 -0.2(6) . . . . ?
C17 N1 N2 B1 -175.6(5) . . . . ?
C9 C4 C5 C6 0.9(9) . . . . ?
C9 C8 C7 C6 1.4(10) . . . . ?
C8 C7 C6 C5 -0.5(11) . . . . ?
C32 C33 C34 Os1 54.1(5) . . . . ?
C32 C33 C34 C35 0.2(8) . . . . ?
C15 C10 C11 C12 -2.0(9) . . . . ?
C15 C14 C13 C12 1.2(11) . . . . ?
C22 N3 N4 C24 0.8(6) . . . . ?
C22 N3 N4 B1 -171.2(5) . . . . ?
C11 C10 C15 C14 1.9(9) . . . . ?
C11 C12 C13 C14 -1.3(11) . . . . ?
C27 N5 N6 C29 0.5(6) . . . . ?
C27 N5 N6 B1 172.8(5) . . . . ?
C20 C19 C18 C17 179.1(6) . . . . ?
C25 C24 C23 C22 -178.5(7) . . . . ?
C30 C29 C28 C27 179.9(7) . . . . ?
C16 C17 C18 C19 -178.1(6) . . . . ?
B1 N6 C29 C28 -172.6(5) . . . . ?
B1 N6 C29 C30 8.5(10) . . . . ?
B1 N4 C24 C23 170.0(5) . . . . ?
B1 N4 C24 C25 -10.7(10) . . . . ?
B1 N2 C19 C18 175.3(5) . . . . ?
B1 N2 C19 C20 -4.2(9) . . . . ?
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
10.4515 -0.9423 1.3355 -0.2324 -0.9726 0.0092
-10.4515 0.9423 -1.3355 0.2324 0.9726 -0.0092
-5.2794 5.1198 9.5495 0.0104 0.0536 0.9985
5.2794 -5.1198 -9.5495 -0.0104 -0.0536 -0.9985
5.3743 -2.7877 -11.4553 0.3117 -0.0055 -0.9502
-5.3743 2.7877 11.4553 -0.3117 0.0055 0.9502
1.9732 7.4728 -5.3143 0.9785 -0.0251 0.2049
-1.9732 -7.4728 5.3143 -0.9785 0.0251 -0.2049
