Thiocarbonylphosphorane and arsorane ligands.
Burt, Liam K.; Hill, Anthony F.; Jones, Stephanie L.; Chemical communications (Cambridge, England) 58 (2022) 11091–11094; doi:10.1039/d2cc03747e

data_7130692
_publ_section_title
;
 Thiocarbonylphosphorane and arsorane ligands.
;
_journal_issue                   79
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11091
_journal_page_last               11094
_journal_paper_doi               10.1039/d2cc03747e
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C31 H35 B N6 O2 P S W, F6 P, 2(C2 H3 N)'
_chemical_formula_sum            'C35 H41 B F6 N8 O2 P2 S W'
_chemical_formula_weight         1008.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-25
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-19 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.4520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1710(2)
_cell_length_b                   13.29580(10)
_cell_length_c                   22.8330(3)
_cell_measurement_reflns_used    15995
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6210
_cell_measurement_theta_min      4.6000
_cell_volume                     4184.05(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     18.00 106.00   1.00    4.00    --   36.95  38.00-180.00   88
  2  \w    -30.00  54.00   1.00    4.00    --   36.95 -57.00-180.00   84
  3  \w      6.00  76.00   1.00    4.00    --   36.95 -99.00 120.00   70
  4  \w      6.00  76.00   1.00    4.00    --   36.95 -99.00   0.00   70
  5  \w     20.00 104.00   1.00    4.00    --   36.95  57.00 -60.00   84
  6  \w      6.00  33.00   1.00    4.00    --   36.95  84.00-129.61   27
  7  \w    -34.00  66.00   1.00    4.00    --   36.95 -19.00   0.00  100
  8  \w     41.00 109.00   1.00   25.00    --  111.00-111.00 -90.00   68
  9  \w     43.00 138.00   1.00   25.00    --  111.00 -77.00 -90.00   95
 10  \w     42.00 130.00   1.00   25.00    --  111.00 -38.00 -60.00   88
 11  \w     41.00 109.00   1.00   25.00    --  111.00-111.00  90.00   68
 12  \w    103.00 178.00   1.00   25.00    --  111.00  77.00  30.00   75
 13  \w     42.00 130.00   1.00   25.00    --  111.00 -38.00  90.00   88
 14  \w     42.00 130.00   1.00   25.00    --  111.00 -38.00  30.00   88
 15  \w     41.00 109.00   1.00   25.00    --  111.00-111.00   0.00   68
 16  \w     42.00 130.00   1.00   25.00    --  111.00 -38.00-150.00   88
 17  \w     92.00 178.00   1.00   25.00    --  111.00  38.00-180.00   86
 18  \w     43.00 138.00   1.00   25.00    --  111.00 -77.00  90.00   95
 19  \w     41.00 109.00   1.00   25.00    --  111.00-111.00-180.00   68
 20  \w     65.00 178.00   1.00   25.00    --  111.00  12.00 -60.00  113
 21  \w     18.00 106.00   1.00    4.00    --   36.95  38.00  90.00   88
 22  \w      4.00  30.00   1.00    4.00    --   36.95  88.00  -8.66   26
 23  \w      3.00  29.00   1.00    4.00    --   36.95  90.00  40.73   26
;
_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      -0.1110082000
_diffrn_orient_matrix_UB_12      -0.0089666000
_diffrn_orient_matrix_UB_13      -0.0218949000
_diffrn_orient_matrix_UB_21      -0.0034080000
_diffrn_orient_matrix_UB_22      -0.0632723000
_diffrn_orient_matrix_UB_23      0.0559767000
_diffrn_orient_matrix_UB_31      -0.0126538000
_diffrn_orient_matrix_UB_32      0.0966228000
_diffrn_orient_matrix_UB_33      0.0346583000
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33037
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.074
_diffrn_reflns_theta_min         3.875
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.905
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O, MeCN'
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+4.9390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7020
_reflns_number_total             7935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03747e2.cif
_cod_data_source_block           lb068_faces
_cod_depositor_comments
'Adding full bibliography for 7130690--7130692.cif.'
_cod_database_code               7130692
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C35H41BF6N8O2P2SW
_chemical_oxdiff_usercomment     'MeCN/Et2O layer @ -20 degC, argon 2 weeks'
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C41(H41A,H41B,
 H41C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              28762
_shelx_hkl_checksum              56065
_ins_header
;
TITL LB068_faces in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  14.170981  13.295752  22.833001  90.0000 103.4525  90.0000
ZERR    4.00   0.000209   0.000140   0.000325   0.0000   0.0014   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O F P S W
UNIT 140.00 164.00 4.00 32.00 8.00 24.00 8.00 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 1.306
_oxdiff_exptl_absorpt_empirical_full_min 0.770
_publcif_funding_html
;
;