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_7130691
_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 Mo N6 O2 P, F6 P, C4 H8 O'
_chemical_formula_sum            'C40 H45 B F6 Mo N6 O3 P2'
_chemical_formula_weight         940.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-19
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2022-06-19 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.26730(10)
_cell_length_b                   18.2717(2)
_cell_length_c                   25.4905(2)
_cell_measurement_reflns_used    12308
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5640
_cell_measurement_theta_min      4.2250
_cell_volume                     4315.12(7)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_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      6.00  76.00   1.00    8.88    --   36.95 -99.00 150.00   70
  2  \w      6.00  76.00   1.00    8.88    --   36.95 -99.00 -60.00   70
  3  \w     20.00 104.00   1.00    8.88    --   36.95  57.00-120.00   84
  4  \w      6.00  76.00   1.00    8.88    --   36.95 -99.00  60.00   70
  5  \w     41.00 109.00   1.00   37.50    --  111.00-111.00  90.00   68
  6  \w     44.00 131.00   1.00   37.50    --  111.00 -64.00 120.00   87
  7  \w     91.00 178.00   1.00   37.50    --  111.00  64.00-180.00   87
  8  \w    104.00 178.00   1.00   37.50    --  111.00 111.00 -90.00   74
  9  \w     43.00 128.00   1.00   37.50    --  111.00 -50.00-150.00   85
 10  \w     42.00 106.00   1.00   37.50    --  111.00 -92.00  90.00   64
 11  \w     41.00 157.00   1.00   37.50    --  111.00 -12.00-180.00  116
 12  \w   -104.00 -20.00   1.00    8.88    --  -36.95 -57.00  60.00   84
 13  \w     18.00 106.00   1.00    8.88    --   36.95  38.00-180.00   88
 14  \w     18.00 106.00   1.00    8.88    --   36.95  38.00   0.00   88
 15  \w     86.00 153.00   1.00   37.50    --  111.00  25.00 -90.00   67
 16  \w     86.00 178.00   1.00   37.50    --  111.00  25.00   0.00   92
;
_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      0.1436786000
_diffrn_orient_matrix_UB_12      -0.0424586000
_diffrn_orient_matrix_UB_13      0.0010719000
_diffrn_orient_matrix_UB_21      0.0539583000
_diffrn_orient_matrix_UB_22      0.0466283000
_diffrn_orient_matrix_UB_23      0.0468198000
_diffrn_orient_matrix_UB_31      -0.0639981000
_diffrn_orient_matrix_UB_32      -0.0559580000
_diffrn_orient_matrix_UB_33      0.0382296000
_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  0.0252
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25513
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.854
_diffrn_reflns_theta_min         4.230
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.797
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.397
_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 light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       needle
_exptl_crystal_F_000             1928
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, n-hexane'
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8599
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+3.4654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7762
_reflns_number_total             8599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03747e2.cif
_cod_data_source_block           lb073_faces
_cod_depositor_comments
'Adding full bibliography for 7130690--7130692.cif.'
_cod_database_code               7130691
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H43BF6MoN6O3P2
_chemical_oxdiff_usercomment     'THF/n-hex liquid liquid argon, r.t. 2 weeks,'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C50 = O3-C54
 1.44 with sigma of 0.02
 C50-C51 = C53-C54
 1.53 with sigma of 0.02
 C51-C53
 1.54 with sigma of 0.02
 O3-C51 = O3-C53 = C50-C53 = C51-C54
 2.38 with sigma of 0.04
 C51-C54 \\sim C50-C53
 with sigma of 0.04
 C50-C51 \\sim C51-C53 \\sim C53-C54
 with sigma of 0.02
 O3-C50 \\sim O3-C54
 with sigma of 0.02
 O3-C51 \\sim O3-C53
 with sigma of 0.04
 C51-C53 \\sim C52-C53
 with sigma of 0.02
 C50-C51 \\sim C50-C52
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O3 \\sim C50 \\sim C53 \\sim C54 \\sim C51: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C51) = Uanis(C52)
5. Rigid body (RIGU) restrains
 O3, C50, C53, C54, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C52)=Sof(H52A)=Sof(H52B)=1-FVAR(1)
 Sof(C51)=Sof(H51B)=Sof(H51A)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 B1(H1)
7.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C53(H53A,H53B), C54(H54A,H54B), C51(H51B,H51A), C52(H52A,H52B)
7.c 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)
7.d 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)
;
_shelx_res_checksum              9619
_shelx_hkl_checksum              52437
_ins_header
;
TITL LB073_faces in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   9.267250  18.271706  25.490540  90.0000  91.3313  90.0000
ZERR    4.00   0.000072   0.000192   0.000238   0.0000   0.0007   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O F P Mo
UNIT 160.00 172.00 4.00 24.00 12.00 24.00 8.00 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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.835