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

data_7713925
_publ_section_title
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 Isonitrile \m2-Carbido Complexes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02649C
_journal_year                    2023
_chemical_formula_moiety         'C38 H45 B Br N8 O2 Pt W'
_chemical_formula_sum            'C41 H46 B Br Cl3 N8 O2 Pt W'
_chemical_formula_weight         1258.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc27zl1w
_audit_creation_date             2019-11-27
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 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                90
_cell_angle_beta                 90.7607(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.9197(3)
_cell_length_b                   13.80583(17)
_cell_length_c                   34.4091(6)
_cell_measurement_reflns_used    13902
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.0160
_cell_measurement_theta_min      4.9470
_cell_volume                     9936.9(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.986
_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    -33.00  52.00   1.00    7.50    --   36.18 -38.00 150.00   85
  2  \w     27.00  90.00   1.00    7.50    --   36.18-125.00   0.00   63
  3  \w    -24.00  23.00   1.00    7.50    --   36.18 -57.00-120.00   47
  4  \w     28.00  90.00   1.00    7.50    --   36.18-125.00-180.00   62
  5  \w     18.00  51.00   1.00    7.50    --   36.18  38.00 -30.00   33
  6  \w     55.00 105.00   1.00    7.50    --   36.18  38.00 -30.00   50
  7  \w     18.00 105.00   1.00    7.50    --   36.18  38.00 120.00   87
  8  \w     28.00  53.00   1.00    7.50    --   36.18 -57.00-120.00   25
  9  \w     19.00 101.00   1.00    7.50    --   36.18  57.00  30.00   82
 10  \w     42.00 109.00   1.00   20.00    --  109.99-111.00 150.00   67
 11  \w     81.00 126.00   1.00   20.00    --  109.99 -45.00   0.00   45
 12  \w     97.00 157.00   1.00   20.00    --  109.99  61.00  60.00   60
 13  \w     46.00 109.00   1.00   20.00    --  109.99-111.00 -30.00   63
 14  \w     43.00 121.00   1.00   20.00    --  109.99 -45.00-180.00   78
 15  \w     43.00  68.00   1.00   20.00    --  109.99 -45.00   0.00   25
 16  \w     42.00 127.00   1.00   20.00    --  109.99 -45.00 -90.00   85
 17  \w     45.00 106.00   1.00   20.00    --  109.99 -95.00-150.00   61
 18  \w     42.00 127.00   1.00   20.00    --  109.99 -45.00  90.00   85
 19  \w     42.00 178.00   1.00   20.00    --  109.99   0.00-150.00  136
 20  \w     61.00 133.00   1.00   20.00    --  109.99 -77.00 -30.00   72
;
_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      0.0022434000
_diffrn_orient_matrix_UB_12      0.0322670000
_diffrn_orient_matrix_UB_13      0.0428487000
_diffrn_orient_matrix_UB_21      0.0461044000
_diffrn_orient_matrix_UB_22      -0.0838698000
_diffrn_orient_matrix_UB_23      0.0096852000
_diffrn_orient_matrix_UB_31      0.0574089000
_diffrn_orient_matrix_UB_32      0.0660885000
_diffrn_orient_matrix_UB_33      -0.0087187000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            29091
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.201
_diffrn_reflns_theta_min         3.836
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45085
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       block
_exptl_crystal_F_000             4856
_refine_diff_density_max         1.374
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+54.7743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8154
_reflns_number_total             9812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02649c2.cif
_cod_data_source_block           lb027
_cod_database_code               7713925
_publcif_datablock.id            {15d804c9-f992-4745-b1e7-b956b7d0bf33}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C41 H46 O2 N5 B1 Br1 Cl3 Pt1 W1'
_chemical_oxdiff_usercomment     'CHCl3/nhex vap diff, 5 degC'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C16(H16), C23(H23), C26(H26), C33(H33), C36(H36)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8B,H8A,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C25(H25A,H25B,
 H25C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C38(H38A,
 H38B,H38C)
;
_shelx_res_checksum              67222
_shelx_fab_checksum              42086
_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 1.889
_oxdiff_exptl_absorpt_empirical_full_min 0.698
_publcif_funding_html
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;