Arsolyl-Supported Intermetallic Dative Bonding
Kirk, Ryan M.; Hill, Anthony; Chemical Science  (2022) –; doi:10.1039/D2SC01200F

data_1566913
_publ_section_title
;
 Arsolyl-Supported Intermetallic Dative Bonding
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01200F
_journal_year                    2022
_chemical_formula_moiety         'C23 H12 As Co F10 O3 Pt'
_chemical_formula_sum            'C23 H12 As Co F10 O3 Pt'
_chemical_formula_weight         855.27
_chemical_properties_physical    Air-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-24 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.18910(10)
_cell_length_b                   12.75590(10)
_cell_length_c                   21.0227(2)
_cell_measurement_reflns_used    6805
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.7250
_cell_measurement_theta_min      5.9050
_cell_volume                     2464.18(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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     32.00 104.00   1.00    1.00    --   36.98  57.00  30.00   72
  2  \w     36.00  74.00   1.00    1.00    --   36.98 -99.00  90.00   38
  3  \w     26.00  87.00   1.00    1.00    --   36.98  38.00  90.00   61
  4  \w    -22.00  35.00   1.00    1.00    --   36.98 -38.00  90.00   57
  5  \w    103.00 147.00   1.00    4.00    --  111.00  77.00  30.00   44
  6  \w     74.00 125.00   1.00    4.00    --  111.00 -50.00-180.00   51
  7  \w    109.00 137.00   1.00    4.00    --  111.00 -77.00 -60.00   28
  8  \w     93.00 175.00   1.00    4.00    --  111.00  38.00-180.00   82
  9  \w     41.00 109.00   1.00    4.00    --  111.00-111.00  30.00   68
 10  \w     66.00 101.00   1.00    4.00    --  111.00-111.00   0.00   35
 11  \w     96.00 145.00   1.00    4.00    --  111.00  50.00 120.00   49
 12  \w    114.00 160.00   1.00    4.00    --  111.00 111.00-150.00   46
 13  \w     79.00 120.00   1.00    4.00    --  111.00 -50.00  30.00   41
 14  \w     50.00  80.00   1.00    4.00    --  111.00 -64.00-180.00   30
 15  \w     63.00  95.00   1.00    4.00    --  111.00 -77.00 -60.00   32
;
_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      -0.0125492000
_diffrn_orient_matrix_UB_12      -0.0990677000
_diffrn_orient_matrix_UB_13      0.0416279000
_diffrn_orient_matrix_UB_21      -0.0016129000
_diffrn_orient_matrix_UB_22      0.0686914000
_diffrn_orient_matrix_UB_23      0.0602847000
_diffrn_orient_matrix_UB_31      -0.1670502000
_diffrn_orient_matrix_UB_32      0.0067559000
_diffrn_orient_matrix_UB_33      -0.0036834000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8725
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.745
_diffrn_reflns_theta_min         4.054
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.190
_exptl_absorpt_correction_T_max  0.23775
_exptl_absorpt_correction_T_min  0.14128
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent intense orange'
_exptl_crystal_density_diffrn    2.305
_exptl_crystal_description       prism
_exptl_crystal_F_000             1608
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.067
_exptl_crystal_size_rad          0.078
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Flack x determined using 1703 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0516P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.628
_reflns_Friedel_fraction_full    0.859
_reflns_Friedel_fraction_max     0.820
_reflns_number_gt                4529
_reflns_number_total             4597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01200f2.cif
_cod_data_source_block           rmk_209_f_scale
_cod_database_code               1566913
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H12As1Co1O3Pt1F10
_chemical_oxdiff_usercomment     'Et2O evap at -30'
_shelx_estimated_absorpt_t_max   0.375
_shelx_estimated_absorpt_t_min   0.086
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_ins_header
;
TITL RMK_209_F_scale in P2(1)2(1)2(1) 
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184   9.189136  12.755857  21.022699  90.0000  90.0000  90.0000
ZERR    4.00   0.000063   0.000092   0.000160   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 O F Co As Pt
UNIT 92.00 48.00 12.00 40.00 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 2.195
_oxdiff_exptl_absorpt_empirical_full_min 0.663