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_7710825
_publ_section_title
;
 Heterobimetallic \m2-halocarbyne complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01558G
_journal_year                    2022
_chemical_formula_moiety         'C44 H46 B Cl Mo N6 O2 P2 Pt'
_chemical_formula_sum            'C44 H46 B Cl Mo N6 O2 P2 Pt'
_chemical_formula_weight         1090.10
_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             2021-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-15 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                83.317(2)
_cell_angle_beta                 89.918(2)
_cell_angle_gamma                87.946(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6762(2)
_cell_length_b                   13.5205(4)
_cell_length_c                   15.4074(4)
_cell_measurement_reflns_used    12369
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5900
_cell_measurement_theta_min      5.7660
_cell_volume                     2207.48(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.992
_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    -32.00  55.00   1.00    1.00    --   37.05 -38.00 150.00   87
  2  \w     18.00  53.00   1.00    1.00    --   37.05  38.00 120.00   35
  3  \w     76.00 107.00   1.00    1.00    --   37.05  19.00  90.00   31
  4  \w     59.00 106.00   1.00    1.00    --   37.05  38.00 120.00   47
  5  \w      8.00  76.00   1.00    1.00    --   37.05 -99.00 120.00   68
  6  \w     36.00  89.00   1.00    1.00    --   37.05-125.00  30.00   53
  7  \w     26.00 106.00   1.00    1.00    --   37.05  38.00 -30.00   80
  8  \w      6.00  73.00   1.00    1.00    --   37.05 -99.00 -90.00   67
  9  \w      8.00  62.00   1.00    1.00    --   37.05  19.00  90.00   54
 10  \w     41.00 136.00   1.00    1.00    --  111.00 -25.00 -90.00   95
 11  \w    149.00 178.00   1.00    1.00    --  111.00  77.00-120.00   29
 12  \w    106.00 140.00   1.00    1.00    --  111.00  77.00-120.00   34
 13  \w     68.00 146.00   1.00    1.00    --  111.00 178.00 150.00   78
 14  \w     49.00 109.00   1.00    1.00    --  111.00-111.00 -90.00   60
 15  \w    141.00 178.00   1.00    1.00    --  111.00  50.00   0.00   37
 16  \w     42.00 121.00   1.00    1.00    --  111.00 -38.00  90.00   79
 17  \w     46.00  73.00   1.00    1.00    --  111.00 -50.00 -90.00   27
 18  \w     81.00 106.00   1.00    1.00    --  111.00 -92.00 -60.00   25
 19  \w     42.00 127.00   1.00    1.00    --  111.00 -25.00-180.00   85
 20  \w     76.00 118.00   1.00    1.00    --  111.00 -50.00 -90.00   42
 21  \w     83.00 109.00   1.00    1.00    --  111.00-111.00  60.00   26
 22  \w     51.00  78.00   1.00    1.00    --  111.00-111.00  60.00   27
 23  \w     43.00  70.00   1.00    1.00    --  111.00 -92.00 -60.00   27
 24  \w     44.00 153.00   1.00    1.00    --  111.00 -12.00  30.00  109
 25  \w    105.00 176.00   1.00    1.00    --  111.00 111.00-150.00   71
 26  \w     58.00 109.00   1.00    1.00    --  111.00-111.00 150.00   51
 27  \w     46.00 101.00   1.00    1.00    --  111.00 -92.00-180.00   55
 28  \w     76.00 138.00   1.00    1.00    --  111.00 -77.00-150.00   62
 29  \w     46.00  73.00   1.00    1.00    --  111.00 -77.00-150.00   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      -0.1371182000
_diffrn_orient_matrix_UB_12      -0.0265997000
_diffrn_orient_matrix_UB_13      0.0194205000
_diffrn_orient_matrix_UB_21      0.0425163000
_diffrn_orient_matrix_UB_22      -0.1088619000
_diffrn_orient_matrix_UB_23      0.0291919000
_diffrn_orient_matrix_UB_31      0.0154910000
_diffrn_orient_matrix_UB_32      0.0248936000
_diffrn_orient_matrix_UB_33      0.0943702000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16573
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.117
_diffrn_reflns_theta_min         4.121
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.755
_exptl_absorpt_correction_T_max  0.585
_exptl_absorpt_correction_T_min  0.261
_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 red'
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, n-hexane'
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.137
_refine_diff_density_max         1.999
_refine_diff_density_min         -2.410
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8625
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0183P)^2^+6.2904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8509
_reflns_number_total             8625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lb053_faces
_cod_database_code               7710825
_publcif_datablock.id            {9ea03f56-cf93-4c8d-a949-ab32f06a7117}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C44H46BClMoN6O2P2Pt
_chemical_oxdiff_usercomment     'Vap Diff. THF/Hex. r.t.'
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C9, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C9 \\sim C10: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
4. Others
 Sof(Cl2)=Sof(O3)=1-FVAR(1)
 Sof(Cl1)=Sof(O2)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 B1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), 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)
5.d 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 LB053_faces in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.676220  13.520523  15.407381  83.3168  89.9179  87.9456
ZERR    2.00   0.000249   0.000445   0.000447   0.0025   0.0022   0.0023
LATT  1
SFAC C H B N O P Cl Mo Pt
UNIT 88.00 92.00 2.00 12.00 4.00 4.00 2.00 2.00 2.00
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 1.271
_oxdiff_exptl_absorpt_empirical_full_min 0.888
_publcif_funding_html
;
;