Isonitrile μ2-Carbido Complexes
Hill, Anthony; Burt, Liam K.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02649C

data_7713929
_publ_section_title
;
 Isonitrile \m2-Carbido Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02649C
_journal_year                    2023
_chemical_formula_moiety         'C45 H46 B Br N7 O2 P Pt W, C H2 Cl2'
_chemical_formula_sum            'C46 H48 B Br Cl2 N7 O2 P Pt W'
_chemical_formula_weight         1302.44
_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_block_doi                 10.5517/ccdc.csd.cc27zl2x
_audit_creation_date             2021-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-21 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                88.182(2)
_cell_angle_beta                 77.516(2)
_cell_angle_gamma                82.340(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4191(2)
_cell_length_b                   15.8501(4)
_cell_length_c                   16.1962(4)
_cell_measurement_reflns_used    14464
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.7000
_cell_measurement_theta_min      4.8280
_cell_volume                     2339.74(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.997
_diffrn_measured_fraction_theta_max 0.996
_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     20.00 104.00   1.00    2.19    --   37.19  57.00 -30.00   84
  2  \w     18.00 106.00   1.00    2.19    --   37.19  38.00-150.00   88
  3  \w    -32.00  56.00   1.00    2.19    --   37.19 -38.00-150.00   88
  4  \w     27.00  91.00   1.00    2.19    --   37.19-125.00-120.00   64
  5  \w     17.00 104.00   1.00    2.19    --   37.19  65.00  40.90   87
  6  \w      4.00  30.00   1.00    2.19    --   37.19  88.00 140.83   26
  7  \w     27.00  91.00   1.00    2.19    --   37.19-125.00  60.00   64
  8  \w     18.00 106.00   1.00    2.19    --   37.19  38.00 150.00   88
  9  \w     42.00 130.00   1.00   11.00    --  111.00 -38.00 120.00   88
 10  \w     42.00 130.00   1.00   11.00    --  111.00 -38.00 -30.00   88
 11  \w     43.00 128.00   1.00   11.00    --  111.00 -50.00 -60.00   85
 12  \w     43.00 138.00   1.00   11.00    --  111.00 -77.00   0.00   95
 13  \w     41.00 109.00   1.00   11.00    --  111.00-111.00  90.00   68
 14  \w     61.00 146.00   1.00   11.00    --  111.00 178.00  90.00   85
 15  \w     41.00 109.00   1.00   11.00    --  111.00-111.00-180.00   68
 16  \w     41.00 136.00   1.00   11.00    --  111.00 -25.00  30.00   95
 17  \w     41.00 109.00   1.00   11.00    --  111.00-111.00 -30.00   68
 18  \w     94.00 178.00   1.00   11.00    --  111.00  50.00 -90.00   84
 19  \w    103.00 178.00   1.00   11.00    --  111.00  77.00  90.00   75
 20  \w     43.00 138.00   1.00   11.00    --  111.00 -77.00-180.00   95
 21  \w     42.00 178.00   1.00   11.00    --  111.00   0.00  60.00  136
 22  \w    -32.00  56.00   1.00    2.19    --   37.19 -38.00 120.00   88
 23  \w    -32.00  56.00   1.00    2.19    --   37.19 -38.00  30.00   88
 24  \w     10.00  42.00   1.00    2.19    --   37.19  77.00 -62.33   32
 25  \w    -30.00  54.00   1.00    2.19    --   37.19 -57.00 -60.00   84
 26  \w      4.00  30.00   1.00    2.19    --   37.19  88.00-126.67   26
 27  \w      4.00  30.00   1.00    2.19    --   37.19  88.00 -86.54   26
 28  \w     65.00 178.00   1.00   11.00    --  111.00  12.00-150.00  113
 29  \w     92.00 178.00   1.00   11.00    --  111.00  38.00  30.00   86
 30  \w     92.00 178.00   1.00   11.00    --  111.00  38.00   0.00   86
 31  \w     86.00 178.00   1.00   11.00    --  111.00  25.00 -30.00   92
 32  \w     92.00 178.00   1.00   11.00    --  111.00  38.00  60.00   86
 33  \w     92.00 178.00   1.00   11.00    --  111.00  38.00-120.00   86
 34  \w     92.00 178.00   1.00   11.00    --  111.00  38.00-150.00   86
 35  \w     91.00 178.00   1.00   11.00    --  111.00  64.00  60.00   87
 36  \w     94.00 178.00   1.00   11.00    --  111.00  50.00 120.00   84
 37  \w     91.00 178.00   1.00   11.00    --  111.00  64.00-120.00   87
 38  \w     92.00 178.00   1.00   11.00    --  111.00  38.00-180.00   86
 39  \w     86.00 178.00   1.00   11.00    --  111.00  25.00 120.00   92
 40  \w     18.00 106.00   1.00    2.19    --   37.19  38.00 -60.00   88
 41  \w      4.00  30.00   1.00    2.19    --   37.19  89.00  69.07   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      -0.0847213000
_diffrn_orient_matrix_UB_12      -0.0060618000
_diffrn_orient_matrix_UB_13      -0.0705511000
_diffrn_orient_matrix_UB_21      0.0541384000
_diffrn_orient_matrix_UB_22      0.0825948000
_diffrn_orient_matrix_UB_23      -0.0399021000
_diffrn_orient_matrix_UB_31      0.1357672000
_diffrn_orient_matrix_UB_32      -0.0525291000
_diffrn_orient_matrix_UB_33      -0.0540505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34638
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         3.961
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.727
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.238
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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 orange'
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       plate
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.039
_refine_diff_density_max         3.457
_refine_diff_density_min         -2.086
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         8849
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0698P)^2^+3.2684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7651
_reflns_number_total             8849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02649c2.cif
_cod_data_source_block           lb045_faces
_cod_database_code               7713929
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         BBrC46Cl2N7O2PPtW
_chemical_oxdiff_usercomment     'Vap diff, dcm/nHex, 5 degC o/n'
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Pt1, W1, C1
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Pt1 \\sim W1 \\sim C1: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C17(H17), 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),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C),
 C017(H01A,H01B,H01C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C27(H27A,H27B,
 H27C)
;
_ins_header
;
TITL LB045_faces in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.419088  15.850121  16.196242  88.1815  77.5162  82.3400
ZERR    2.00   0.000227   0.000421   0.000404   0.0021   0.0021   0.0021
LATT  1
SFAC C B N O P Cl Br W Pt
UNIT 92.00 2.00 14.00 4.00 2.00 4.00 2.00 2.00 2.00
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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.689