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

data_7709145
_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         'C31 H35 As B N6 O2 W, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C33 H37 As B Cl2 F3 N6 O5 S W'
_chemical_formula_weight         1027.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9239(2)
_cell_length_b                   19.4360(6)
_cell_length_c                   25.6769(11)
_cell_measurement_reflns_used    2494
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.6510
_cell_measurement_theta_min      2.8690
_cell_volume                     3954.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.964
_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   -104.00  -9.00   1.00   30.00    --  -36.03 -77.00 -90.00   95
  2  \w    -51.00  30.00   1.00   30.00    --  -36.03  57.00-180.00   81
  3  \w     39.00 109.00   1.00   70.00    --  107.33 -95.00-180.00   70
  4  \w     95.00 140.00   1.00   70.00    --  107.33  45.00-150.00   45
  5  \w    100.00 167.00   1.00   70.00    --  107.33 111.00  30.00   67
  6  \w     50.00 127.00   1.00   70.00    --  107.33 -30.00  60.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1115872000
_diffrn_orient_matrix_UB_12      -0.0020215000
_diffrn_orient_matrix_UB_13      -0.0491079000
_diffrn_orient_matrix_UB_21      0.1579913000
_diffrn_orient_matrix_UB_22      0.0116587000
_diffrn_orient_matrix_UB_23      0.0338314000
_diffrn_orient_matrix_UB_31      0.0206625000
_diffrn_orient_matrix_UB_32      -0.0783628000
_diffrn_orient_matrix_UB_33      0.0063722000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8183
_diffrn_reflns_point_group_measured_fraction_full 0.817
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.998
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.347
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Flack x determined using 1493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.040(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.449
_reflns_Friedel_fraction_full    0.593
_reflns_Friedel_fraction_max     0.558
_reflns_number_gt                5440
_reflns_number_total             6113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03790k2.cif
_cod_data_source_block           Compound_6
_cod_depositor_comments
'Adding full bibliography for 7709141--7709146.cif.'
_cod_database_code               7709145
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C32 H35 As B F3 N6 O5 S W'
_chemical_oxdiff_usercomment     'Grown from evaporation of DCM solution'
_reflns_odcompleteness_completeness 99.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 B(H)
1.b Secondary CH2 refined with riding coordinates:
 C98(H98A,H98B)
1.c Aromatic/amide H refined with riding coordinates:
 C62(H62), C15(H15), C12(H12), C6(H6), C16(H16), C13(H13), C9(H9), C14(H14),
 C7(H7), C10(H10), C8(H8), C57(H57), C52(H52)
1.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C50(H50A,H50B,
 H50C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              85009
_shelx_hkl_checksum              21734
_ins_header
;
TITL 37C_scale in P2(1)2(1)2(1) 
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184   7.923874  19.435995  25.676925  90.0000  90.0000  90.0000
ZERR    4.00   0.000217   0.000592   0.001098   0.0000   0.0000   0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H B N O F S As W
UNIT 128.00 140.00 4.00 24.00 20.00 12.00 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 1.120
_oxdiff_exptl_absorpt_empirical_full_min 0.917