Arsinocarbyne reactivity.
Frogley, Benjamin J.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1907–1917; doi:10.1039/d1dt03790k

data_7709144
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -102.00 -19.00   1.00    7.00    --  -36.03 -38.00-120.00   83
  2  \w    -78.00  31.00   1.00    7.00    --  -36.03   0.00  90.00  109
  3  \w    -51.00  20.00   1.00    7.00    --  -36.03  57.00 120.00   71
  4  \w      7.00  73.00   1.00    7.00    --   36.03 -99.00-150.00   66
  5  \w     33.00  96.00   1.00    7.00    --   36.03-136.00  54.00   63
  6  \w    117.00 159.00   1.00   30.00    --  105.15  61.00  30.00   42
  7  \w     38.00 114.00   1.00   30.00    --  105.15 -45.00-180.00   76
  8  \w     44.00 164.00   1.00   30.00    --  105.15   0.00  30.00  120
  9  \w     38.00 115.00   1.00   30.00    --  105.15 -45.00 -30.00   77
 10  \w     60.00 109.00   1.00   30.00    --  105.15-111.00 -30.00   49
 11  \w     58.00 123.00   1.00   30.00    --  105.15 -45.00-120.00   65
 12  \w     53.00 105.00   1.00   30.00    --  105.15 -95.00-150.00   52
 13  \w     37.00 123.00   1.00   30.00    --  105.15 -45.00  90.00   86
 14  \w     50.00 106.00   1.00   30.00    --  105.15 -95.00 120.00   56
 15  \w    103.00 173.00   1.00   30.00    --  105.15  77.00-120.00   70
 16  \w     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       '\w 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/[\s^2^(Fo^2^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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'
_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)
;
_shelx_res_checksum              74160
_shelx_hkl_checksum              34016
_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