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_7710831
_publ_section_title
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 Heterobimetallic \m2-halocarbyne complexes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01558G
_journal_year                    2022
_chemical_formula_moiety         'C54 H52 B Cl N6 O2 P2 Pt W'
_chemical_formula_sum            'C54 H52 B Cl N6 O2 P2 Pt W'
_chemical_formula_weight         1304.15
_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             2020-10-27
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2022-05-15 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.4300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.56140(10)
_cell_length_b                   22.6311(2)
_cell_length_c                   23.3107(3)
_cell_measurement_reflns_used    17095
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5690
_cell_measurement_theta_min      3.8270
_cell_volume                     4989.59(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.983
_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   -104.00 -20.00   1.00    5.91    --  -37.19 -57.00-120.00   84
  2  \w     27.00  91.00   1.00    5.91    --   37.19-125.00  30.00   64
  3  \w    -30.00  54.00   1.00    5.91    --   37.19 -57.00-180.00   84
  4  \w      6.00  76.00   1.00    5.91    --   37.19 -99.00 120.00   70
  5  \w     18.00 106.00   1.00    5.91    --   37.19  38.00 120.00   88
  6  \w    103.00 178.00   1.00   23.64    --  111.00  77.00  60.00   75
  7  \w    103.00 178.00   1.00   23.64    --  111.00  77.00 -90.00   75
  8  \w    103.00 178.00   1.00   23.64    --  111.00  77.00   0.00   75
  9  \w     43.00 128.00   1.00   23.64    --  111.00 -50.00  30.00   85
 10  \w     43.00 128.00   1.00   23.64    --  111.00 -50.00 -60.00   85
 11  \w     42.00 106.00   1.00   23.64    --  111.00 -92.00 -30.00   64
 12  \w     41.00 109.00   1.00   23.64    --  111.00-111.00  60.00   68
 13  \w    103.00 178.00   1.00   23.64    --  111.00  77.00  30.00   75
 14  \w   -104.00 -20.00   1.00    5.91    --  -37.19 -57.00  60.00   84
 15  \w   -104.00 -20.00   1.00    5.91    --  -37.19 -57.00 -30.00   84
 16  \w   -105.00 -57.00   1.00    5.91    --  -37.19-155.00-177.00   48
 17  \w    -30.00  54.00   1.00    5.91    --   37.19 -57.00  30.00   84
 18  \w     19.00 106.00   1.00    5.91    --   37.19  39.00-158.00   87
 19  \w     94.00 178.00   1.00   23.64    --  111.00  50.00 -30.00   84
 20  \w     65.00 178.00   1.00   23.64    --  111.00  12.00-180.00  113
 21  \w     86.00 113.00   1.00   23.64    --  111.00  25.00-120.00   27
;
_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      -0.0494375000
_diffrn_orient_matrix_UB_12      0.0629647000
_diffrn_orient_matrix_UB_13      -0.0180306000
_diffrn_orient_matrix_UB_21      0.1448210000
_diffrn_orient_matrix_UB_22      0.0245862000
_diffrn_orient_matrix_UB_23      0.0271925000
_diffrn_orient_matrix_UB_31      0.0555821000
_diffrn_orient_matrix_UB_32      -0.0080096000
_diffrn_orient_matrix_UB_33      -0.0583337000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35306
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.965
_diffrn_reflns_theta_min         3.834
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.845
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.497
_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    1.736
_exptl_crystal_description       plate
_exptl_crystal_F_000             2552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, n-hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.139
_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     623
_refine_ls_number_reflns         9939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0495P)^2^+8.5100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8797
_reflns_number_total             9939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           en002_faces
_cod_database_code               7710831
_publcif_datablock.id            {5fb79d76-a625-41f0-8d38-e28c7c2a664d}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C54H52BClN6O2P2PtW
_chemical_oxdiff_usercomment     'Picked from flask of material, carbido?'
_shelx_estimated_absorpt_t_max   0.624
_shelx_estimated_absorpt_t_min   0.410
_reflns_odcompleteness_completeness 99.53
_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 Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
 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),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C71(H71), C72(H72), C73(H73),
  C74(H74), C75(H75)
2.b 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)
;
_ins_header
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TITL EN002_faces in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   9.561418  22.631084  23.310674  90.0000  98.4300  90.0000
ZERR    4.00   0.000094   0.000237   0.000255   0.0000   0.0010   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 216.00 208.00 4.00 24.00 8.00 8.00 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 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.813
_publcif_funding_html
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