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

data_7709146
_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         'C30 H32 As Au2 B Cl2 N6 O2 W, 1.5(C H Cl3)'
_chemical_formula_sum            'C31.5 H33.5 As Au2 B Cl6.5 N6 O2 W'
_chemical_formula_weight         1422.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-11 deposited with the CCDC.	2021-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.357(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.5578(9)
_cell_length_b                   16.1269(6)
_cell_length_c                   23.1612(9)
_cell_measurement_reflns_used    11691
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4530
_cell_measurement_theta_min      3.7060
_cell_volume                     8443.1(6)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -86.00  12.00   1.00   32.00    --  -11.30 -37.00-120.00   98
  2  \w    -89.00 -62.00   1.00   32.00    --  -11.30-178.00  90.00   27
  3  \w     42.00  71.00   1.00   32.00    --   11.61 178.00-180.00   29
  4  \w    -61.00 -22.00   1.00   32.00    --   11.61 -57.00-150.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0264202000
_diffrn_orient_matrix_UB_12      0.0147623000
_diffrn_orient_matrix_UB_13      0.0053788000
_diffrn_orient_matrix_UB_21      0.0074665000
_diffrn_orient_matrix_UB_22      -0.0207654000
_diffrn_orient_matrix_UB_23      0.0281700000
_diffrn_orient_matrix_UB_31      0.0151784000
_diffrn_orient_matrix_UB_32      0.0358141000
_diffrn_orient_matrix_UB_33      0.0140397000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20825
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48085
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.237
_exptl_crystal_description       block
_exptl_crystal_F_000             5288
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.149
_refine_diff_density_max         1.291
_refine_diff_density_min         -2.385
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         8605
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+72.3197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7479
_reflns_number_total             8605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03790k2.cif
_cod_data_source_block           Compound_5
_cod_depositor_comments
'Adding full bibliography for 7709141--7709146.cif.'
_cod_original_formula_sum        'C31.50 H33.50 As Au2 B Cl6.50 N6 O2 W'
_cod_database_code               7709146
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H32 As Au2 B Cl2 N6 O2 W'
_chemical_oxdiff_usercomment     d/p
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C10 \\sim C15 \\sim C15A \\sim C14A \\sim C14 \\sim C13 \\sim C12 \\sim C11:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
3. Others
 Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=1-FVAR(1)
 Sof(C15)=Sof(H15)=Sof(H13)=Sof(C14)=Sof(H14)=FVAR(1)
 Fixed Sof: Cl6(0.5) Cl7(0.5) Cl9(0.5) C32(0.5) H32(0.5)
4.a Ternary CH refined with riding coordinates:
 C31(H31), C32(H32)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C28(H28), C11(H11), C9(H9), C8(H8), C23(H23), C5(H5), C12(H12),
 C7(H7), C15(H15), C6(H6), C13(H13), C13(H13A), C14(H14), C14A(H14A), C15A(H15A)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C21(H21A,H21B,
 H21C), C20(H20A,H20B,H20C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              66357
_shelx_hkl_checksum              43616
_ins_header
;
TITL BF136C_scale in C2/c 
REM C2/c (#15 in standard setting)
CELL 0.71073  23.557814  16.126946  23.161187  90.0000 106.3569  90.0000
ZERR    8.00   0.000894   0.000602   0.000861   0.0000   0.0040   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H B N O Cl As W Au
UNIT 240.00 256.00 8.00 48.00 16.00 16.00 8.00 8.00 16.00
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 1.939
_oxdiff_exptl_absorpt_empirical_full_min 0.594