Heterobimetallic μ2-halocarbyne complexes
Burt, Liam K.; Dewhurst, Rian D.; Hill, Anthony F.; Kong, Richard Y.; Nahon, Emily E.; Onn, Chee S.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01558G

data_7710829
_publ_section_title
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 Heterobimetallic \m2-halocarbyne complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01558G
_journal_year                    2022
_chemical_formula_moiety         'C37 H37 B Cl N6 O3 P Pt W'
_chemical_formula_sum            'C37 H37 B Cl N6 O3 P Pt W'
_chemical_formula_weight         1069.89
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-07
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2022-05-15 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.07980(10)
_cell_length_b                   16.51380(10)
_cell_length_c                   15.43220(10)
_cell_measurement_reflns_used    23503
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.7250
_cell_measurement_theta_min      3.9740
_cell_volume                     3836.22(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     27.00  90.00   1.00    1.00    --   36.95-125.00 150.00   63
  2  \w     20.00 104.00   1.00    1.00    --   36.95  57.00  60.00   84
  3  \w     20.00 104.00   1.00    1.00    --   36.95  57.00   0.00   84
  4  \w     18.00 106.00   1.00    1.00    --   36.95  38.00-150.00   88
  5  \w    103.00 178.00   1.00    2.53    --  111.00  77.00  30.00   75
  6  \w     43.00 138.00   1.00    2.53    --  111.00 -77.00  30.00   95
  7  \w     94.00 178.00   1.00    2.53    --  111.00  50.00   0.00   84
  8  \w     86.00 178.00   1.00    2.53    --  111.00  25.00 120.00   92
  9  \w     41.00 109.00   1.00    2.53    --  111.00-111.00  90.00   68
 10  \w     43.00 128.00   1.00    2.53    --  111.00 -50.00 -30.00   85
 11  \w    103.00 178.00   1.00    2.53    --  111.00  77.00 120.00   75
 12  \w     43.00 128.00   1.00    2.53    --  111.00 -50.00  30.00   85
 13  \w     42.00 106.00   1.00    2.53    --  111.00 -92.00   0.00   64
 14  \w    -54.00  30.00   1.00    1.00    --  -36.95  57.00  60.00   84
 15  \w     18.00 106.00   1.00    1.00    --   36.95  38.00 -60.00   88
 16  \w    -30.00  54.00   1.00    1.00    --   36.95 -57.00 -90.00   84
 17  \w    -21.00  64.00   1.00    1.00    --   36.95 -77.00-150.00   85
 18  \w     86.00 178.00   1.00    2.53    --  111.00  25.00 -60.00   92
 19  \w     92.00 178.00   1.00    2.53    --  111.00  38.00 -30.00   86
 20  \w     42.00 106.00   1.00    2.53    --  111.00 -92.00-150.00   64
 21  \w     86.00 178.00   1.00    2.53    --  111.00  25.00  60.00   92
 22  \w     65.00 178.00   1.00    2.53    --  111.00  12.00 -90.00  113
 23  \w     41.00 109.00   1.00    2.53    --  111.00-111.00-150.00   68
 24  \w    104.00 178.00   1.00    2.53    --  111.00 111.00  60.00   74
 25  \w     92.00 178.00   1.00    2.53    --  111.00  38.00-180.00   86
 26  \w     20.00  89.00   1.00    1.00    --   36.95  57.00 120.00   69
;
_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      0.0253694000
_diffrn_orient_matrix_UB_12      -0.0575387000
_diffrn_orient_matrix_UB_13      0.0760193000
_diffrn_orient_matrix_UB_21      -0.0030152000
_diffrn_orient_matrix_UB_22      -0.0723411000
_diffrn_orient_matrix_UB_23      -0.0631495000
_diffrn_orient_matrix_UB_31      0.0991241000
_diffrn_orient_matrix_UB_32      0.0124952000
_diffrn_orient_matrix_UB_33      -0.0152604000
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37185
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         3.924
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.572
_exptl_absorpt_correction_T_max  0.556
_exptl_absorpt_correction_T_min  0.213
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (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 pink'
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_description       prism
_exptl_crystal_F_000             2056
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, n-hexane'
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0237P)^2^+5.9167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6747
_reflns_number_total             7008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lbx356_faces_new
_cod_database_code               7710829
_publcif_datablock.id            {6c4045dd-d463-4c4c-931f-c0754c51e597}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C37H37BClN6O3PPtW
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(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 Aromatic/amide H refined with riding coordinates:
 C35(H35), C21(H21), C44(H44), C34(H34), C6(H6), C45(H45), C31(H31), C22(H22),
 C41(H41), C43(H43), C42(H42), C32(H32), C33(H33), C25(H25), C23(H23), C11(H11),
  C24(H24), C16(H16)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C),
 C18(H18A,H18B,H18C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              37969
_ins_header
;
TITL LBX356_faces_NEW in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  15.079806  16.513755  15.432163  90.0000  93.4043  90.0000
ZERR    4.00   0.000104   0.000092   0.000087   0.0000   0.0006   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H B N O P Cl W Pt
UNIT 148.00 148.00 4.00 24.00 12.00 4.00 4.00 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 1.717
_oxdiff_exptl_absorpt_empirical_full_min 0.577
_publcif_funding_html
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;