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_7705258
_publ_section_title
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 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         'C34 H45 B N6 O2 P Pt W, F6 P'
_chemical_formula_sum            'C34 H45 B F6 N6 O2 P2 Pt W'
_chemical_formula_weight         1135.45
_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
_audit_creation_date             2020-07-26
_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                 101.691(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0989(4)
_cell_length_b                   23.4132(6)
_cell_length_c                   24.3451(8)
_cell_measurement_reflns_used    6657
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.6800
_cell_measurement_theta_min      3.7890
_cell_volume                     8427.8(4)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.827
_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    -51.00  30.00   1.00  180.00    --   15.42 -57.00-150.00   81
  2  \w    -20.00  49.00   1.00  180.00    --   15.42 -99.00   0.00   69
  3  \w    -47.00  -4.00   1.00  180.00    --   15.42 -77.00 150.00   43
;
_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      0.0292785000
_diffrn_orient_matrix_UB_12      -0.0216236000
_diffrn_orient_matrix_UB_13      -0.0063119000
_diffrn_orient_matrix_UB_21      0.0101506000
_diffrn_orient_matrix_UB_22      0.0171223000
_diffrn_orient_matrix_UB_23      -0.0219719000
_diffrn_orient_matrix_UB_31      0.0366219000
_diffrn_orient_matrix_UB_32      0.0125373000
_diffrn_orient_matrix_UB_33      0.0190380000
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.1054
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35063
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.311
_diffrn_reflns_theta_min         3.265
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.183
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89222
_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_density_diffrn    1.790
_exptl_crystal_description       needle
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.022
_refine_diff_density_max         2.170
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         19108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0339P)^2^+48.2942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12461
_reflns_number_total             19108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02737e2.cif
_cod_data_source_block           Compound_6
_cod_depositor_comments
'Adding full bibliography for 7705254--7705258.cif.'
_cod_database_code               7705258
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H47 B1 F6 N6 O2 P2 Pt1 W1'
_chemical_oxdiff_usercomment     'DCM ethanol hexane'
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.305
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(C28A) = Uanis(C27A)
Uanis(C28) = Uanis(C31)
Uanis(C30) = Uanis(C29)
Uanis(C29A) = Uanis(C30A) = Uanis(C34A) = Uanis(C33A)
Uanis(F1A) = Uanis(F6A)
Uanis(C6) = Uanis(C16)
Uanis(C2A) = Uanis(C3A)
3.a Ternary CH refined with riding coordinates:
 C31A(H31A), C27A(H27A), B1(H1), C32A(H32A), C27(H27), C28A(H28A), C32(H32),
 B1A(H1A), C31(H31), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C30A(H30A,H30B), C33A(H33A,H33B), C33(H33C,H33D), C34A(H34A,H34B), C30(H30C,
 H30D), C29A(H29A,H29B), C34(H34C,H34D), C29(H29C,H29D)
3.c Aromatic/amide H refined with riding coordinates:
 C16A(H16A), C26(H26), C11(H11), C6A(H6A), C22A(H22A), C22(H22), C6(H6),
 C16(H16), C24A(H24A), C11A(H11A), C26A(H26A), C25A(H25A), C24(H24), C23(H23),
 C25(H25), C23A(H23A)
3.d Idealised Me refined as rotating group:
 C20A(H20A,H20B,H20C), C14A(H14A,H14B,H14C), C9(H9A,H9B,H9C), C19A(H19A,H19B,
 H19C), C20(H20D,H20E,H20F), C13A(H13A,H13B,H13C), C3AA(H3AA,H3AB,H3AC), C4(H4A,
 H4B,H4C), C8A(H8AA,H8AB,H8AC), C19(H19D,H19E,H19F), C14(H14D,H14E,H14F),
 C13(H13D,H13E,H13F), C18A(H18A,H18B,H18C), C9A(H9AA,H9AB,H9AC), C8(H8A,H8B,
 H8C), C18(H18D,H18E,H18F)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 1007.2 Ang^3^ [12.0%]
Total electron count / cell = 178.2
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_ins_header
;
TITL CO_AO_Pt COD_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  15.098945  23.413237  24.345131  90.0000 101.6908  90.0000
ZERR    8.00   0.000424   0.000580   0.000757   0.0000   0.0028   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O F P W Pt
UNIT 272.00 376.00 8.00 48.00 16.00 48.00 16.00 8.00 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 1.151
_oxdiff_exptl_absorpt_empirical_full_min 0.823