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_7710819
_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         'C36 H44 B2 Cl2 N12 O4 Pt W2'
_chemical_formula_sum            'C36 H44 B2 Cl2 N12 O4 Pt W2'
_chemical_formula_weight         1364.14
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
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2022-05-15 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                73.274(6)
_cell_angle_beta                 64.083(7)
_cell_angle_gamma                83.109(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4275(7)
_cell_length_b                   10.6735(7)
_cell_length_c                   11.3340(9)
_cell_measurement_reflns_used    3443
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.3870
_cell_measurement_theta_min      4.6970
_cell_volume                     1086.56(15)
_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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.979
_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    -29.00   2.00   1.00    2.57    --   37.45 -57.00  60.00   31
  2  \w    -29.00  56.00   1.00    2.57    --   37.45 -38.00  90.00   85
  3  \w     81.00 108.00   1.00    2.57    --   37.45  19.00-120.00   27
  4  \w     29.00  91.00   1.00    2.57    --   37.45-125.00  90.00   62
  5  \w    -31.00  54.00   1.00    2.57    --   37.45 -38.00 -60.00   85
  6  \w     27.00  88.00   1.00    2.57    --   37.45-125.00-180.00   61
  7  \w      3.00  30.00   1.00    2.57    --   37.45 -57.00  60.00   27
  8  \w     33.00  74.00   1.00    2.57    --   37.45 -99.00 -90.00   41
  9  \w     29.00  63.00   1.00    2.57    --   37.45  19.00-120.00   34
 10  \w     29.00  79.00   1.00    2.57    --   37.45-125.00   0.00   50
 11  \w     19.00 106.00   1.00    2.57    --   37.45  38.00 -90.00   87
 12  \w     45.00 128.00   1.00   10.28    --  111.00 -50.00  90.00   83
 13  \w     78.00 126.00   1.00   10.28    --  111.00 -25.00 120.00   48
 14  \w     73.00 108.00   1.00   10.28    --  111.00-111.00 -60.00   35
 15  \w     81.00 108.00   1.00   10.28    --  111.00-111.00   0.00   27
 16  \w     42.00  74.00   1.00   10.28    --  111.00-111.00   0.00   32
 17  \w    107.00 171.00   1.00   10.28    --  111.00 111.00-120.00   64
 18  \w    135.00 162.00   1.00   10.28    --  111.00  50.00 150.00   27
 19  \w    100.00 160.00   1.00   10.28    --  111.00  50.00-180.00   60
 20  \w     70.00 109.00   1.00   10.28    --  111.00-111.00-180.00   39
 21  \w     47.00  74.00   1.00   10.28    --  111.00 -77.00 -30.00   27
 22  \w     76.00 126.00   1.00   10.28    --  111.00 -77.00 -30.00   50
 23  \w     96.00 172.00   1.00   10.28    --  111.00  38.00  60.00   76
 24  \w     82.00 128.00   1.00   10.28    --  111.00 -50.00 -30.00   46
 25  \w     67.00 109.00   1.00   10.28    --  111.00-111.00 120.00   42
 26  \w     65.00 127.00   1.00   10.28    --  111.00 -25.00-120.00   62
 27  \w     46.00  79.00   1.00   10.28    --  111.00 -50.00 -30.00   33
 28  \w     44.00 114.00   1.00   10.28    --  111.00 -50.00-150.00   70
 29  \w     71.00 124.00   1.00   10.28    --  111.00 -77.00 150.00   53
 30  \w     96.00 178.00   1.00   10.28    --  111.00  38.00 -60.00   82
;
_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      0.1384451000
_diffrn_orient_matrix_UB_12      0.0498550000
_diffrn_orient_matrix_UB_13      -0.1274815000
_diffrn_orient_matrix_UB_21      0.0787772000
_diffrn_orient_matrix_UB_22      -0.1224000000
_diffrn_orient_matrix_UB_23      0.0455716000
_diffrn_orient_matrix_UB_31      -0.0401271000
_diffrn_orient_matrix_UB_32      -0.0724414000
_diffrn_orient_matrix_UB_33      -0.0788317000
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7640
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.446
_diffrn_reflns_theta_min         4.325
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.037
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.399
_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 dark red'
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_description       plate
_exptl_crystal_F_000             646
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3, n-hexane'
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.198
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0363P)^2^+2.3840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3579
_reflns_number_total             4291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           en001_facesraw
_cod_database_code               7710819
_publcif_datablock.id            {6c2ecb06-2d9b-49d8-88b3-b1696b74d8ff}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C36H47B2Cl2N12O4PtW2
_chemical_oxdiff_usercomment     'Vap. diff. @ 5degC, o/n, CHCl3/nHex'
_shelx_estimated_absorpt_t_max   0.549
_shelx_estimated_absorpt_t_min   0.289
_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. Others
 Fixed Sof: Pt1(0.4) Cl1(0.5) O1(0.5) O2(0.5) C2(0.5) Cl2(0.5) O3(0.5) O4(0.5)
 C4(0.5) Pt2(0.1)
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C17(H17)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              3300
_ins_header
;
TITL EN001_facesraw in P1 
REM P1 (#1 in standard setting)
CELL 1.54184  10.427524  10.673459  11.334016  73.2744  64.0827  83.1089
ZERR    1.00   0.000657   0.000719   0.000853   0.0063   0.0068   0.0054
LATT -1
SFAC C H B N O Cl W Pt
UNIT 36.00 47.00 2.00 12.00 4.00 2.00 2.00 1.00
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 1.292
_oxdiff_exptl_absorpt_empirical_full_min 0.746
_publcif_funding_html
;
;