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

data_7709142
_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, 2(C H Cl3)'
_chemical_formula_sum            'C62 H66 As2 B2 Cl8 N12 O4 Pt W2'
_chemical_formula_weight         2061.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-01 deposited with the CCDC.	2021-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                60.653(9)
_cell_angle_beta                 72.213(8)
_cell_angle_gamma                88.996(7)
_cell_formula_units_Z            1
_cell_length_a                   10.3361(10)
_cell_length_b                   14.4715(11)
_cell_length_c                   14.7530(14)
_cell_measurement_reflns_used    1670
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.5040
_cell_measurement_theta_min      4.5710
_cell_volume                     1808.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.985
_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    -50.00  18.00   1.00   20.00    --  -36.03  57.00 -30.00   68
  2  \w    -84.00  27.00   1.00   20.00    --  -36.03   0.00 -60.00  111
  3  \w   -102.00 -17.00   1.00   20.00    --  -36.03 -38.00  90.00   85
  4  \w     28.00  85.00   1.00   20.00    --   36.03-125.00 -90.00   57
  5  \w     27.00  88.00   1.00   20.00    --   36.03-125.00  90.00   61
  6  \w     55.00 106.00   1.00   80.00    --  105.15 -95.00 -90.00   51
  7  \w    103.00 172.00   1.00   80.00    --  105.15  77.00-120.00   69
  8  \w     37.00 118.00   1.00   80.00    --  105.15 -45.00-150.00   81
  9  \w    103.00 173.00   1.00   80.00    --  105.15  77.00 -90.00   70
 10  \w     36.00 109.00   1.00   80.00    --  105.15-111.00 120.00   73
 11  \w    105.00 174.00   1.00   80.00    --  105.15  45.00 -30.00   69
 12  \w     36.00 100.00   1.00   80.00    --  105.15 -95.00-150.00   64
 13  \w     50.00 144.00   1.00   80.00    --  105.15 -15.00 -90.00   94
 14  \w     36.00 101.00   1.00   80.00    --  105.15 -95.00   0.00   65
 15  \w    125.00 170.00   1.00   80.00    --  105.15  77.00   0.00   45
 16  \w     50.00 113.00   1.00   80.00    --  105.15 -61.00 -30.00   63
 17  \w    122.00 175.00   1.00   80.00    --  105.15 111.00 -60.00   53
;
_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      0.1203839000
_diffrn_orient_matrix_UB_12      0.0226109000
_diffrn_orient_matrix_UB_13      -0.1042678000
_diffrn_orient_matrix_UB_21      -0.1023351000
_diffrn_orient_matrix_UB_22      0.0116676000
_diffrn_orient_matrix_UB_23      -0.0606932000
_diffrn_orient_matrix_UB_31      0.0131809000
_diffrn_orient_matrix_UB_32      0.1210646000
_diffrn_orient_matrix_UB_33      -0.0409624000
_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  0.0826
_diffrn_reflns_av_unetI/netI     0.1912
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9905
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.893
_exptl_crystal_description       needle
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.680
_refine_diff_density_min         -2.186
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3780
_reflns_number_total             6296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03790k2.cif
_cod_data_source_block           Compound_4a
_cod_depositor_comments
'Adding full bibliography for 7709141--7709146.cif.'
_cod_original_cell_volume        1808.2(3)
_cod_database_code               7709142
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H64 As2 B2 Cl2 N12 O4 Pt W2'
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.475
_reflns_odcompleteness_completeness 94.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.55
_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:
 B1(H1), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C11(H11), C18(H18), C14(H14), C23(H23), C9(H9), C5(H5), C28(H28),
 C7(H7), C15(H15), C12(H12), C8(H8), C6(H6)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C30(H30A,H30B,
 H30C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              68297
_shelx_hkl_checksum              11511
_ins_header
;
TITL BF163Etrans_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.336120  14.471465  14.753006  60.6534  72.2129  88.9959
ZERR    2.00   0.000958   0.001098   0.001364   0.0087   0.0082   0.0068
LATT  1
SFAC C H B N O Cl As W Pt
UNIT 120.00 128.00 4.00 24.00 8.00 4.00 4.00 4.00 2.00
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 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.740