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

data_7709143
_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         'C60 H64 As2 B2 Cl2 N12 O4 Pt W2'
_chemical_formula_sum            'C60 H64 As2 B2 Cl2 N12 O4 Pt W2'
_chemical_formula_weight         1822.38
_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             2021-08-18
_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                 97.722(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6734(6)
_cell_length_b                   10.6507(3)
_cell_length_c                   33.0022(11)
_cell_measurement_reflns_used    3168
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.6640
_cell_measurement_theta_min      5.0310
_cell_volume                     6504.1(4)
_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 0.962
_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   -105.00 -21.00   1.00   20.00    --  -36.03 -38.00 120.00   84
  2  \w    -76.00  -6.00   1.00   20.00    --  -36.03 125.00  30.00   70
  3  \w     38.00  84.00   1.00   20.00    --   36.03-125.00 -60.00   46
  4  \w     31.00  89.00   1.00   20.00    --   36.03  57.00   0.00   58
  5  \w     54.00 144.00   1.00   60.00    --  105.15 -15.00 120.00   90
  6  \w     37.00 106.00   1.00   60.00    --  105.15 -95.00-150.00   69
  7  \w     94.00 165.00   1.00   60.00    --  105.15  61.00 -30.00   71
  8  \w     39.00 106.00   1.00   60.00    --  105.15-111.00  30.00   67
  9  \w    106.00 173.00   1.00   60.00    --  105.15  77.00  90.00   67
 10  \w     42.00 117.00   1.00   60.00    --  105.15 -77.00  60.00   75
;
_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      -0.0367578000
_diffrn_orient_matrix_UB_12      0.0109734000
_diffrn_orient_matrix_UB_13      -0.0445049000
_diffrn_orient_matrix_UB_21      -0.0095459000
_diffrn_orient_matrix_UB_22      0.1421667000
_diffrn_orient_matrix_UB_23      0.0058479000
_diffrn_orient_matrix_UB_31      0.0742044000
_diffrn_orient_matrix_UB_32      0.0236331000
_diffrn_orient_matrix_UB_33      -0.0142088000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            10468
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.904
_diffrn_reflns_theta_min         4.780
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50656
_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    1.861
_exptl_crystal_description       needle
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.595
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0303P)^2^+32.9052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4671
_reflns_number_total             6028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03790k2.cif
_cod_data_source_block           Compound_4b
_cod_depositor_comments
'Adding full bibliography for 7709141--7709146.cif.'
_cod_database_code               7709143
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H64 As2 B2 Cl2 N12 O4 Pt W2'
_reflns_odcompleteness_completeness 98.73
_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.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C5(H5), C15(H15), C6(H6), C18(H18), C13(H13), C7(H7), C23(H23),
 C8(H8), C28(H28), C9(H9), C14(H14), C12(H12)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C16(H16A,H16B,
 H16C), C25(H25A,H25B,H25C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              87979
_shelx_hkl_checksum              37053
_ins_header
;
TITL BF163E2_scale in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  18.673380  10.650748  33.002192  90.0000  97.7221  90.0000
ZERR    4.00   0.000572   0.000342   0.001115   0.0000   0.0031   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H B N O Cl As W Pt
UNIT 240.00 256.00 8.00 48.00 16.00 8.00 8.00 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 1.692
_oxdiff_exptl_absorpt_empirical_full_min 0.746