Metal coordination of phosphoniocarbynes.
Onn, Chee S.; Hill, Anthony F.; Olding, Angus; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12731–12741; doi:10.1039/d0dt02737e

data_7705255
_publ_section_title
;
 Metal coordination of phosphoniocarbynes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12731
_journal_page_last               12741
_journal_paper_doi               10.1039/d0dt02737e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C46 H55 B N8 O2 P Pt W, F6 P, C H Cl3'
_chemical_formula_sum            'C47 H56 B Cl3 F6 N8 O2 P2 Pt W'
_chemical_formula_weight         1437.03
_chemical_name_systematic        Compound_8
_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   mixed
_audit_creation_date             2020-07-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-08-05 deposited with the CCDC.	2020-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.001(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5808(4)
_cell_length_b                   14.4490(4)
_cell_length_c                   22.7627(6)
_cell_measurement_reflns_used    9479
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.9890
_cell_measurement_theta_min      3.8260
_cell_volume                     5445.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.834
_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    -11.00  33.00   1.00   47.12    --   15.57  77.00  60.00   44
  2  \w     11.00  72.00   1.00   47.12    --   15.57  57.00 120.00   61
  3  \w    -50.00  32.00   1.00   47.12    --   15.57 -57.00 -60.00   82
  4  \w    -61.00 -35.00   1.00   47.12    --  -16.59 -38.00 120.00   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      -0.0416897000
_diffrn_orient_matrix_UB_12      -0.0074396000
_diffrn_orient_matrix_UB_13      -0.0069693000
_diffrn_orient_matrix_UB_21      0.0042684000
_diffrn_orient_matrix_UB_22      -0.0469100000
_diffrn_orient_matrix_UB_23      0.0088460000
_diffrn_orient_matrix_UB_31      -0.0088027000
_diffrn_orient_matrix_UB_32      0.0124910000
_diffrn_orient_matrix_UB_33      0.0291005000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.834
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24477
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.266
_diffrn_reflns_theta_min         3.328
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       plate
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.692
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.322
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         12383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0124P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9139
_reflns_number_total             12383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02737e2.cif
_cod_data_source_block           co_ao5_ptcod-mesnc_scale
_cod_depositor_comments
'Adding full bibliography for 7705254--7705258.cif.'
_cod_database_code               7705255
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H54 B1 F6 N8 O2 P2 Pt1 W1'
_chemical_oxdiff_usercomment     'DCM hexane'
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C3) = Uanis(C2)
3.a Ternary CH refined with riding coordinates:
 C1A(H1A)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C30(H30), C11(H11), C42(H42), C32(H32), C26(H26), C22(H22),
 C40(H40), C23(H23), C24(H24), C25(H25)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C20(H20A,H20B,H20C),
 C19(H19A,H19B,H19C), C46(H46A,H46B,H46C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C),
  C13(H13A,H13B,H13C), C34(H34A,H34B,H34C), C44(H44A,H44B,H44C), C35(H35A,H35B,
 H35C), C45(H45A,H45B,H45C), C36(H36A,H36B,H36C)
;
_ins_header
;
TITL CO-AO-4-29-F1-PtCOD-MesNC_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  16.580780  14.448997  22.762662  90.0000  93.0013  90.0000
ZERR    4.00   0.000400   0.000411   0.000575   0.0000   0.0025   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O F P W Pt
UNIT 184.00 216.00 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 1.768
_oxdiff_exptl_absorpt_empirical_full_min 0.412