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

data_7713927
_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         'C46 H48 B Br N7 O2 P Pt W, C H Cl3'
_chemical_formula_sum            'C47 H49 B Br Cl3 N7 O2 P Pt W'
_chemical_formula_weight         1350.91
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc27zkzs
_audit_creation_date             2021-01-28
_audit_creation_method
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Olex2 1.2
;
_audit_update_record
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2021-05-21 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
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_cell_angle_alpha                91.074(2)
_cell_angle_beta                 103.031(2)
_cell_angle_gamma                93.835(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5314(3)
_cell_length_b                   16.2298(5)
_cell_length_c                   16.3030(5)
_cell_measurement_reflns_used    8899
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5140
_cell_measurement_theta_min      3.9690
_cell_volume                     2450.02(13)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.968
_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   -103.00 -20.00   1.00    5.04    --  -36.95 -57.00 -60.00   83
  2  \w     33.00  90.00   1.00    5.04    --   36.95-125.00 -30.00   57
  3  \w    -30.00  54.00   1.00    5.04    --   36.95 -57.00 150.00   84
  4  \w     18.00  90.00   1.00    5.04    --   36.95  38.00 -60.00   72
  5  \w     19.00  97.00   1.00    5.04    --   36.95  38.00  60.00   78
  6  \w     30.00  90.00   1.00    5.04    --   36.95-125.00 150.00   60
  7  \w     21.00 102.00   1.00    5.04    --   36.95  57.00  90.00   81
  8  \w     43.00 103.00   1.00   19.14    --  111.00 -38.00  60.00   60
  9  \w     46.00 109.00   1.00   19.14    --  111.00-111.00 120.00   63
 10  \w     43.00  85.00   1.00   19.14    --  111.00 -77.00 -60.00   42
 11  \w    105.00 147.00   1.00   19.14    --  111.00 111.00 150.00   42
 12  \w     41.00 108.00   1.00   19.14    --  111.00-111.00  30.00   67
 13  \w     47.00 109.00   1.00   19.14    --  111.00-111.00 -60.00   62
 14  \w     59.00 124.00   1.00   19.14    --  111.00 -38.00 -30.00   65
 15  \w    104.00 130.00   1.00   19.14    --  111.00 -38.00 120.00   26
 16  \w     47.00  91.00   1.00   19.14    --  111.00 -38.00 120.00   44
 17  \w     43.00 130.00   1.00   19.14    --  111.00 -38.00-150.00   87
 18  \w    101.00 150.00   1.00   19.14    --  111.00  64.00-150.00   49
 19  \w    102.00 138.00   1.00   19.14    --  111.00 -77.00 -60.00   36
 20  \w     52.00 137.00   1.00   19.14    --  111.00 -77.00 120.00   85
 21  \w     44.00 174.00   1.00   19.14    --  111.00   0.00   0.00  130
;
_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      0.1458038000
_diffrn_orient_matrix_UB_12      -0.0299270000
_diffrn_orient_matrix_UB_13      0.0466630000
_diffrn_orient_matrix_UB_21      -0.0271032000
_diffrn_orient_matrix_UB_22      -0.0783192000
_diffrn_orient_matrix_UB_23      -0.0578540000
_diffrn_orient_matrix_UB_31      0.0753509000
_diffrn_orient_matrix_UB_32      0.0450783000
_diffrn_orient_matrix_UB_33      -0.0624065000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16050
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.797
_diffrn_reflns_theta_min         3.832
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.671
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.468
_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 yellow'
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       plate
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.803
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0467P)^2^+0.5530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8386
_reflns_number_total             9597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02649c2.cif
_cod_data_source_block           lb039_faces
_cod_database_code               7713927
_publcif_datablock.id            {ea1f09ba-5b52-4342-ac19-53fac3e4039f}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         BrC48Cl3N2O2PPtW
_chemical_oxdiff_usercomment     'ch/nhex vap diff'
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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.a Ternary CH refined with riding coordinates:
 C60(H60)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C23(H23), C26(H26), 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)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,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)
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_ins_header
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TITL LB039_faces in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.531401  16.229830  16.303031  91.0737 103.0311  93.8349
ZERR    2.00   0.000255   0.000471   0.000457   0.0023   0.0023   0.0023
LATT  1
SFAC C N O P Cl Br W Pt
UNIT 96.00 4.00 4.00 2.00 6.00 2.00 2.00 2.00
TREF
HKLF 4
END
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_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 1.239
_oxdiff_exptl_absorpt_empirical_full_min 0.871
_publcif_funding_html
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