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_7130690
_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         'C36 H37 B N6 O2 P S W, F6 P, C7 H8'
_chemical_formula_sum            'C43 H45 B F6 N6 O2 P2 S W'
_chemical_formula_weight         1080.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-19 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.090(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.2847(5)
_cell_length_b                   13.3933(3)
_cell_length_c                   28.4487(5)
_cell_measurement_reflns_used    8096
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.2470
_cell_measurement_theta_min      5.0600
_cell_volume                     9627.6(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.990
_diffrn_measured_fraction_theta_max 0.989
_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     37.00  90.00   1.00    6.61    --   36.18-125.00-150.00   53
  2  \w     25.00  99.00   1.00    6.61    --   36.18  57.00 120.00   74
  3  \w    -29.00  52.00   1.00    6.61    --   36.18 -38.00-180.00   81
  4  \w    -32.00  23.00   1.00    6.61    --   36.18 -38.00 150.00   55
  5  \w    116.00 159.00   1.00   26.41    --  109.99  77.00 120.00   43
  6  \w    104.00 172.00   1.00   26.41    --  109.99  77.00-150.00   68
  7  \w     40.00 108.00   1.00   26.41    --  109.99-111.00 -60.00   68
  8  \w     67.00 107.00   1.00   26.41    --  109.99-111.00 150.00   40
  9  \w     41.00 127.00   1.00   26.41    --  109.99 -30.00-180.00   86
 10  \w    105.00 178.00   1.00   26.41    --  109.99 111.00-180.00   73
 11  \w    104.00 143.00   1.00   26.41    --  109.99 111.00 150.00   39
 12  \w     42.00 126.00   1.00   26.41    --  109.99 -45.00  90.00   84
;
_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      -0.0096726000
_diffrn_orient_matrix_UB_12      -0.1110543000
_diffrn_orient_matrix_UB_13      -0.0119371000
_diffrn_orient_matrix_UB_21      -0.0194587000
_diffrn_orient_matrix_UB_22      0.0291980000
_diffrn_orient_matrix_UB_23      -0.0500035000
_diffrn_orient_matrix_UB_31      0.0570397000
_diffrn_orient_matrix_UB_32      -0.0090644000
_diffrn_orient_matrix_UB_33      -0.0169696000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            16010
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         3.648
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.033
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.222
_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    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             4320
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, toluene'
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.068
_refine_diff_density_max         2.760
_refine_diff_density_min         -2.727
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1217P)^2^+66.2284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7942
_reflns_number_total             8711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03747e2.cif
_cod_data_source_block           lb047_faces
_cod_depositor_comments
'Adding full bibliography for 7130690--7130692.cif.'
_cod_database_code               7130690
_publcif_datablock.id            {fc272f2a-115b-49b9-8b31-9de7d3a3be25}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C44H47BCl2F6N6O2P2SW
_chemical_oxdiff_usercomment     'DCM,Tol layering and evap'
_reflns_odcompleteness_completeness 98.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C3)
3. Others
 Fixed Sof: F2(0.33333) F4(0.33333) F6(0.33333) F8(0.33333) F1(0.666)
 F3(0.666) F5(0.666) F7(0.666)
4.a Ternary CH refined with riding coordinates:
 B1(H1)
4.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), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
4.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), C50(H50A,H50B,H50C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_ins_header
;
TITL LB047_faces in I2/a 
REM I2/a (#15 in standard setting)
CELL 1.54184  25.284730  13.393289  28.448676  90.0000  92.0905  90.0000
ZERR    8.00   0.000503   0.000297   0.000549   0.0000   0.0018   0.0000
LATT  2
SYMM -x+1/2, y,-z 
SFAC C H B N O F P S Cl W
UNIT 352.00 376.00 8.00 48.00 16.00 48.00 16.00 8.00 16.00 8.00
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 2.779
_oxdiff_exptl_absorpt_empirical_full_min 0.417
_publcif_funding_html
;
;