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_7705254
_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         'C26 H33 Au B Cl N6 O2 P W, F6 P'
_chemical_formula_sum            'C26 H33 Au B Cl F6 N6 O2 P2 W'
_chemical_formula_weight         1064.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2679(5)
_cell_length_b                   24.0778(19)
_cell_length_c                   24.2183(8)
_cell_measurement_reflns_used    4392
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.0810
_cell_measurement_theta_min      3.7650
_cell_volume                     7153.7(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 1.3 (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 0.816
_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    -48.00  74.00   1.00  144.31    --   13.38   0.00-180.00  122
;
_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      -0.0247138000
_diffrn_orient_matrix_UB_12      0.0219731000
_diffrn_orient_matrix_UB_13      -0.0149692000
_diffrn_orient_matrix_UB_21      -0.0301785000
_diffrn_orient_matrix_UB_22      -0.0195746000
_diffrn_orient_matrix_UB_23      -0.0156231000
_diffrn_orient_matrix_UB_31      -0.0427196000
_diffrn_orient_matrix_UB_32      0.0011937000
_diffrn_orient_matrix_UB_33      0.0197257000
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17300
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.417
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.539
_exptl_absorpt_correction_T_max  0.68345
_exptl_absorpt_correction_T_min  0.67654
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense red'
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_description       plate
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.035
_exptl_crystal_size_rad          0.034
_refine_diff_density_max         4.092
_refine_diff_density_min         -1.936
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7351
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0610P)^2^+133.9816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5361
_reflns_number_total             7351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02737e2.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
'Adding full bibliography for 7705254--7705258.cif.'
_cod_database_code               7705254
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Au1 C26 Cl1 H33 B1 F6 N6 O2 P2 W1'
_chemical_oxdiff_usercomment     'DCM ethanol'
_reflns_odcompleteness_completeness 95.24
_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. Rigid bond restraints
 C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26: within 0.8A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 0.8A
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C11(H11), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
4.b Fitted hexagon refined as free rotating group:
 C21(C22,C23,C24,C25,C26)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C)
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_ins_header
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TITL CO_AO_AuCl_scale_sph corr in Pbca 
REM Pbca (#61 in standard setting)
CELL 0.71073  12.267860  24.077791  24.218345  90.0000  90.0000  90.0000
ZERR    8.00   0.000534   0.001924   0.000807   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H B N O F P Cl W Au
UNIT 208.00 264.00 8.00 48.00 16.00 48.00 16.00 8.00 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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.869