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

data_7713926
_publ_section_title
;
 Isonitrile \m2-Carbido Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02649C
_journal_year                    2023
_chemical_formula_moiety         'C38 H49 B2 N11 O2 Pt W'
_chemical_formula_sum            'C38 H49 B2 N11 O2 Pt W'
_chemical_formula_weight         1092.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-27 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.6300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.99650(10)
_cell_length_b                   24.0347(3)
_cell_length_c                   21.9700(2)
_cell_measurement_reflns_used    14061
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5780
_cell_measurement_theta_min      4.4500
_cell_volume                     4185.11(8)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_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    1.00    --  -37.05 -57.00 -60.00   83
  2  \w    -22.00 102.00   1.00    1.00    --   37.05   0.00 -30.00  124
  3  \w    -31.00  56.00   1.00    1.00    --   37.05 -38.00 -30.00   87
  4  \w     27.00  90.00   1.00    1.00    --   37.05-125.00 -60.00   63
  5  \w    -30.00  48.00   1.00    1.00    --   37.05 -57.00 150.00   78
  6  \w     39.00 105.00   1.00    1.00    --   37.05-150.00 168.00   66
  7  \w     81.00 109.00   1.00    3.44    --  111.00-111.00 150.00   28
  8  \w    131.00 177.00   1.00    3.44    --  111.00  77.00  60.00   46
  9  \w     47.00 105.00   1.00    3.44    --  111.00 -77.00 150.00   58
 10  \w     81.00 129.00   1.00    3.44    --  111.00 -38.00   0.00   48
 11  \w    109.00 177.00   1.00    3.44    --  111.00  77.00  30.00   68
 12  \w    103.00 130.00   1.00    3.44    --  111.00  77.00  60.00   27
 13  \w     42.00  79.00   1.00    3.44    --  111.00 -38.00   0.00   37
 14  \w     62.00 109.00   1.00    3.44    --  111.00-111.00  60.00   47
 15  \w     95.00 176.00   1.00    3.44    --  111.00  50.00  90.00   81
 16  \w     41.00 109.00   1.00    3.44    --  111.00-111.00 -90.00   68
 17  \w     42.00 129.00   1.00    3.44    --  111.00 -38.00 -90.00   87
 18  \w     47.00 122.00   1.00    3.44    --  111.00 -77.00  30.00   75
 19  \w     42.00 130.00   1.00    3.44    --  111.00 -38.00  90.00   88
 20  \w     45.00 131.00   1.00    3.44    --  111.00 -77.00 -90.00   86
 21  \w     68.00 178.00   1.00    3.44    --  111.00   0.00  30.00  110
;
_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      0.0397100000
_diffrn_orient_matrix_UB_12      -0.0626084000
_diffrn_orient_matrix_UB_13      -0.0025962000
_diffrn_orient_matrix_UB_21      -0.1882282000
_diffrn_orient_matrix_UB_22      -0.0123822000
_diffrn_orient_matrix_UB_23      -0.0202031000
_diffrn_orient_matrix_UB_31      0.0275858000
_diffrn_orient_matrix_UB_32      0.0061510000
_diffrn_orient_matrix_UB_33      -0.0677468000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28346
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.989
_diffrn_reflns_theta_min         4.060
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.540
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8341
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7756
_reflns_number_total             8341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02649c2.cif
_cod_data_source_block           lb036_facesanalyt
_cod_database_code               7713926
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H49B2N11O2Pt1W1
_chemical_oxdiff_usercomment     'CHCl3/EtOH vap diff, 5 degC, o/n'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O2, C3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O2 \\sim C3: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
4.a Secondary CH2 refined with riding coordinates:
 B2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C21(H21), C26(H26), C33(H33), C36(H36)
4.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), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C35(H35A,
 H35B,H35C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              19672
_ins_header
;
TITL LB036_facesAnalyt in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   7.996543  24.034682  21.970021  90.0000  97.6298  90.0000
ZERR    4.00   0.000082   0.000257   0.000213   0.0000   0.0009   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O W Pt
UNIT 152.00 196.00 8.00 44.00 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 1.647
_oxdiff_exptl_absorpt_empirical_full_min 0.569