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_7705256
_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         'C52 H66 B2 Cl2 Cu2 N12 O4 P2 W2, 2(F6 P)'
_chemical_formula_sum            'C52 H66 B2 Cl2 Cu2 F12 N12 O4 P4 W2'
_chemical_formula_weight         1862.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                111.350(6)
_cell_angle_beta                 100.699(5)
_cell_angle_gamma                90.294(5)
_cell_formula_units_Z            2
_cell_length_a                   13.3582(8)
_cell_length_b                   16.9977(10)
_cell_length_c                   17.9256(11)
_cell_measurement_reflns_used    6357
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      70.3870
_cell_measurement_theta_min      4.1660
_cell_volume                     3713.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.958
_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    -95.00  26.00   1.00    7.50    --  -35.53   0.00  60.00  121
  2  \w    -52.00  19.00   1.00    7.50    --  -35.53  57.00  90.00   71
  3  \w     27.00  87.00   1.00    7.50    --   35.53-125.00   0.00   60
  4  \w    -30.00  50.00   1.00    7.50    --   35.53 -57.00-150.00   80
  5  \w     11.00  74.00   1.00    7.50    --   35.53 -99.00 150.00   63
  6  \w     40.00 109.00   1.00   30.00    --  105.15-111.00-150.00   69
  7  \w     35.00 126.00   1.00   30.00    --  105.15 -30.00 -90.00   91
  8  \w     49.00 132.00   1.00   30.00    --  105.15 -77.00-120.00   83
  9  \w     89.00 172.00   1.00   30.00    --  105.15  61.00 -60.00   83
 10  \w     36.00 127.00   1.00   30.00    --  105.15 -30.00   0.00   91
 11  \w     48.00  94.00   1.00   30.00    --  105.15 -61.00-180.00   46
 12  \w     95.00 123.00   1.00   30.00    --  105.15 -61.00-180.00   28
 13  \w     36.00 109.00   1.00   30.00    --  105.15-111.00  60.00   73
 14  \w    107.00 173.00   1.00   30.00    --  105.15  77.00 -30.00   66
 15  \w     59.00 132.00   1.00   30.00    --  105.15 -77.00  30.00   73
 16  \w     34.00 134.00   1.00   30.00    --  105.15 -15.00 150.00  100
;
_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      -0.0226294000
_diffrn_orient_matrix_UB_12      -0.0741817000
_diffrn_orient_matrix_UB_13      -0.0834367000
_diffrn_orient_matrix_UB_21      -0.0603883000
_diffrn_orient_matrix_UB_22      -0.0503423000
_diffrn_orient_matrix_UB_23      0.0356374000
_diffrn_orient_matrix_UB_31      -0.0985071000
_diffrn_orient_matrix_UB_32      0.0386322000
_diffrn_orient_matrix_UB_33      -0.0253481000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20370
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.558
_diffrn_reflns_theta_min         3.878
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.381
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
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    1.666
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.052
_refine_diff_density_max         2.837
_refine_diff_density_min         -1.944
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         13639
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0797
_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^)+(0.0456P)^2^+86.2570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9649
_reflns_number_total             13639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02737e2.cif
_cod_data_source_block           Compound_5
_cod_depositor_comments
;
Adding full bibliography for 7705254--7705258.cif.

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C26 H33 B Cl Cu F6 N6 O2 P2 W'
_cod_original_formula_weight         931.17
_cod_original_formula_moiety       '0.5(C52 H66 B2 Cl2 Cu2 N12 O4 P2 W2), F6 P'
_cod_original_formula_units_Z            4
_cod_database_code               7705256
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H48 Cu1 B1 F6 N6 O2 P2 W1'
_chemical_oxdiff_usercomment     D/H
_reflns_odcompleteness_completeness 97.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Restrained distances
 B1A-H1A
 1.1 with sigma of 0.02
3. Rigid bond restraints
 C26, C25, C24, C23, C22, C21
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C18, C17, C16, C15, C14
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C13, C12, C11, C10, C9
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C8, C7, C6, C5, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C26 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 1.7A
C13 \\sim C12 \\sim C11 \\sim C10 \\sim C9: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 1.7A
C8 \\sim C7 \\sim C6 \\sim C5 \\sim C4: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 1.7A
Uanis(N1A) = Uanis(N5A)
5.a Aromatic/amide H refined with riding coordinates:
 C11A(H11A), C26A(H26A), C6A(H6A), C25A(H25A), C16A(H16A), C22A(H22A),
 C23A(H23A), C6(H6), C16(H16), C26(H26), C24A(H24A), C22(H22), C11(H11),
 C25(H25), C23(H23), C24(H24)
5.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C19A(H19A,H19B,H19C), C4A(H4AA,H4AB,H4AC), C9A(H9AA,H9AB,
 H9AC), C8A(H8AA,H8AB,H8AC), C14A(H14A,H14B,H14C), C20A(H20A,H20B,H20C), C9(H9A,
 H9B,H9C), C13A(H13A,H13B,H13C), C14(H14D,H14E,H14F), C18A(H18A,H18B,H18C),
 C8(H8A,H8B,H8C), C19(H19D,H19E,H19F), C18(H18D,H18E,H18F), C13(H13D,H13E,H13F),
  C20(H20D,H20E,H20F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 120 electrons were 
found in a volume of 547 Ang^3^ in 2 voids per unit cell. 
This is consistent with the presence of 2[CHCl3] per 
Asymmetric Unit which account for 464 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_ins_header
;
TITL CO_AO_WCP_CuCl_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  13.358246  16.997692  17.925632 111.3499 100.6986  90.2939
ZERR    4.00   0.000810   0.001030   0.001067   0.0056   0.0050   0.0049
LATT  1
SFAC C H B N O F P Cu W
UNIT 144.00 192.00 4.00 24.00 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 1.667
_oxdiff_exptl_absorpt_empirical_full_min 0.347