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

data_7709141
_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 H47 As B Cl2 Ir N6 O2 W, 2.5(C H Cl3)'
_chemical_formula_sum            'C42.5 H49.5 As B Cl9.5 Ir N6 O2 W'
_chemical_formula_weight         1474.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 106.977(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.5783(7)
_cell_length_b                   18.5015(5)
_cell_length_c                   33.6485(9)
_cell_measurement_reflns_used    4795
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.6410
_cell_measurement_theta_min      4.6570
_cell_volume                     12252.7(7)
_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 0.985
_diffrn_measured_fraction_theta_max 0.963
_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    -91.00 -19.00   1.00   25.00    --  -35.78 -57.00   0.00   72
  2  \w   -102.00 -24.00   1.00   25.00    --  -35.78 -57.00 -60.00   78
  3  \w     19.00  95.00   1.00   25.00    --   35.78  57.00 -90.00   76
  4  \w     46.00  91.00   1.00   25.00    --   35.78  57.00-180.00   45
  5  \w     35.00 144.00   1.00   75.00    --  105.15 -15.00  60.00  109
  6  \w     35.00 127.00   1.00   75.00    --  105.15 -30.00-180.00   92
  7  \w     39.00 123.00   1.00   75.00    --  105.15 -77.00   0.00   84
  8  \w    108.00 160.00   1.00   75.00    --  105.15 111.00-180.00   52
  9  \w     37.00 106.00   1.00   75.00    --  105.15 -95.00 150.00   69
;
_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      -0.0000943000
_diffrn_orient_matrix_UB_12      -0.0309909000
_diffrn_orient_matrix_UB_13      -0.0425029000
_diffrn_orient_matrix_UB_21      0.0776849000
_diffrn_orient_matrix_UB_22      -0.0095500000
_diffrn_orient_matrix_UB_23      0.0159271000
_diffrn_orient_matrix_UB_31      -0.0096380000
_diffrn_orient_matrix_UB_32      -0.0766697000
_diffrn_orient_matrix_UB_33      0.0152384000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18947
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.723
_diffrn_reflns_theta_min         3.834
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72409
_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_density_diffrn    1.599
_exptl_crystal_description       needle
_exptl_crystal_F_000             5704
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.854
_refine_diff_density_min         -2.170
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         11362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0688P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8164
_reflns_number_total             11362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03790k2.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
'Adding full bibliography for 7709141--7709146.cif.'
_cod_original_formula_sum        'C42.50 H49.50 As B Cl9.50 Ir N6 O2 W'
_cod_database_code               7709141
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H49 As B Cl8 Ir N6 O2 W'
_shelx_estimated_absorpt_t_max   0.710
_shelx_estimated_absorpt_t_min   0.328
_reflns_odcompleteness_completeness 98.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Others
 Fixed Sof: Cl10(0.5) H41(0.5)
3.a Ternary CH refined with riding coordinates:
 C42(H42), C43(H43), C41(H41)
3.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C18(H18), C9(H9), C11(H11), C23(H23), C8(H8), C12(H12), C15(H15),
 C5(H5), C7(H7), C6(H6), C13(H13), C14(H14)
3.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C26(H26A,H26B,H26C), C40(H40A,H40B,H40C), C36(H36A,H36B,
 H36C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C25(H25A,H25B,H25C), C37(H37A,
 H37B,H37C), C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68534
_shelx_hkl_checksum              65346
_shelx_fab_checksum              75843
_ins_header
;
TITL BF136D_scale in I2/a 
REM I2/a (#15 in standard setting)
CELL 1.54184  20.578270  18.501509  33.648459  90.0000 106.9770  90.0000
ZERR   11.00   0.000737   0.000521   0.000857   0.0000   0.0033   0.0000
LATT  2
SYMM -x+1/2, y,-z 
SFAC C H B N O Cl As W Ir
UNIT 462.00 539.00 11.00 66.00 22.00 88.00 11.00 11.00 11.00
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 2.211
_oxdiff_exptl_absorpt_empirical_full_min 0.648