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_7710827
_publ_section_title
;
 Heterobimetallic \m2-halocarbyne complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01558G
_journal_year                    2022
_chemical_formula_moiety         '2(C54 H52 B Cl Mo N6 O2 P2 Pt), 2.5(C2 H3 N)'
_chemical_formula_sum            'C113 H111.5 B2 Cl2 Mo2 N14.5 O4 P4 Pt2'
_chemical_formula_weight         2535.12
_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             2021-04-23
_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                71.105(2)
_cell_angle_beta                 80.456(2)
_cell_angle_gamma                78.496(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5638(2)
_cell_length_b                   21.0076(4)
_cell_length_c                   24.0458(5)
_cell_measurement_reflns_used    22075
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6670
_cell_measurement_theta_min      4.1790
_cell_volume                     5383.22(19)
_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 (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 0.995
_diffrn_measured_fraction_theta_max 0.989
_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  89.00   1.00    1.00    --   37.05   0.00 -30.00  121
  2  \w     27.00  78.00   1.00    1.00    --   37.05-125.00 150.00   51
  3  \w     24.00  97.00   1.00    1.00    --   37.05  38.00-180.00   73
  4  \w    -32.00  56.00   1.00    1.00    --   37.05 -38.00 -90.00   88
  5  \w      7.00  71.00   1.00    1.00    --   37.05 -99.00  60.00   64
  6  \w    -30.00  52.00   1.00    1.00    --   37.05 -57.00-180.00   82
  7  \w     38.00  88.00   1.00    1.00    --   37.05-125.00-120.00   50
  8  \w     11.00  76.00   1.00    1.00    --   37.05 -99.00 -60.00   65
  9  \w     44.00 112.00   1.00    4.02    --  111.00 -50.00-150.00   68
 10  \w     77.00 109.00   1.00    4.02    --  111.00-111.00  30.00   32
 11  \w     42.00 116.00   1.00    4.02    --  111.00 -38.00  60.00   74
 12  \w    107.00 135.00   1.00    4.02    --  111.00  77.00 120.00   28
 13  \w    136.00 168.00   1.00    4.02    --  111.00  77.00 120.00   32
 14  \w     46.00 129.00   1.00    4.02    --  111.00 -64.00 -30.00   83
 15  \w     45.00 128.00   1.00    4.02    --  111.00 -38.00 -30.00   83
 16  \w     77.00 104.00   1.00    4.02    --  111.00 -92.00-150.00   27
 17  \w     41.00 109.00   1.00    4.02    --  111.00-111.00   0.00   68
 18  \w     70.00 108.00   1.00    4.02    --  111.00-111.00 -60.00   38
 19  \w     42.00  70.00   1.00    4.02    --  111.00 -92.00-150.00   28
 20  \w     41.00  68.00   1.00    4.02    --  111.00-111.00 -60.00   27
 21  \w     45.00 157.00   1.00    4.02    --  111.00 -12.00 -60.00  112
 22  \w     42.00 136.00   1.00    4.02    --  111.00 -25.00 120.00   94
 23  \w     57.00 109.00   1.00    4.02    --  111.00-111.00 120.00   52
 24  \w     52.00 138.00   1.00    4.02    --  111.00 -77.00 120.00   86
 25  \w     41.00 152.00   1.00    4.02    --  111.00 -12.00-150.00  111
;
_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      0.0319380000
_diffrn_orient_matrix_UB_12      -0.0497103000
_diffrn_orient_matrix_UB_13      -0.0372823000
_diffrn_orient_matrix_UB_21      0.0591959000
_diffrn_orient_matrix_UB_22      0.0540726000
_diffrn_orient_matrix_UB_23      -0.0504633000
_diffrn_orient_matrix_UB_31      0.1190897000
_diffrn_orient_matrix_UB_32      -0.0276246000
_diffrn_orient_matrix_UB_33      0.0265401000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41701
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.124
_diffrn_reflns_theta_min         3.925
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.101
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (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 orange'
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             2534
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, MeCN'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.591
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1303
_refine_ls_number_reflns         20974
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+17.4226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19434
_reflns_number_total             20974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lb050_faces
_cod_original_formula_sum        'C113 H111.50 B2 Cl2 Mo2 N14.50 O4 P4 Pt2'
_cod_database_code               7710827
_publcif_datablock.id            {216c8644-6d6c-4037-8803-df5011f9691b}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C113H111B2Cl2Mo2N14.5O4P4Pt2
_chemical_oxdiff_usercomment     'Vap diff, THF/MeCN, 5 degC o/n'
_reflns_odcompleteness_completeness 98.90
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C84, C85, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C84 \\sim C85 \\sim N10: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C61B) = Uanis(C62B) = Uanis(C63B) = Uanis(C64B)
4. Others
 Fixed Sof: N10(0.5) C85(0.5) C84(0.5) H84A(0.5) H84B(0.5) H84C(0.5)
5.a Ternary CH refined with riding coordinates:
 B1A(H1A), B1B(H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C65B(H65B), C31B(H31B), C21B(H21B), C31A(H31A), C25B(H25B), C6B(H6B),
 C75A(H75A), C35A(H35A), C41A(H41A), C41B(H41B), C6A(H6A), C65A(H65A),
 C51B(H51B), C71A(H71A), C51A(H51A), C55B(H55B), C35B(H35B), C25A(H25A),
 C42A(H42A), C71B(H71B), C16B(H16B), C32A(H32A), C23B(H23B), C16A(H16A),
 C21A(H21A), C75B(H75B), C22B(H22B), C33A(H33A), C64B(H64B), C11A(H11A),
 C61A(H61A), C73A(H73A), C11B(H11B), C72B(H72B), C73B(H73B), C42B(H42B),
 C72A(H72A), C52A(H52A), C24A(H24A), C45A(H45A), C32B(H32B), C53A(H53A),
 C34A(H34A), C55A(H55A), C53B(H53B), C54B(H54B), C52B(H52B), C43A(H43A),
 C24B(H24B), C45B(H45B), C34B(H34B), C33B(H33B), C74A(H74A), C54A(H54A),
 C74B(H74B), C44A(H44A), C23A(H23A), C62A(H62A), C63A(H63A), C64A(H64A),
 C22A(H22A), C43B(H43B), C44B(H44B), C61B(H61B), C63B(H63B), C62B(H62B)
5.c Idealised Me refined as rotating group:
 C14B(H14A,H14B,H14C), C9A(H9AA,H9AB,H9AC), C4B(H4BA,H4BB,H4BC), C4A(H4AA,H4AB,
 H4AC), C9B(H9BA,H9BB,H9BC), C8A(H8AA,H8AB,H8AC), C18A(H18D,H18E,H18F),
 C8B(H8BA,H8BB,H8BC), C18B(H18A,H18B,H18C), C13B(H13A,H13B,H13C), C14A(H14D,
 H14E,H14F), C13A(H13D,H13E,H13F), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C),
 C84(H84A,H84B,H84C)
;
_ins_header
;
TITL LB050_faces in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  11.563793  21.007607  24.045758  71.1053  80.4559  78.4959
ZERR    2.00   0.000189   0.000443   0.000487   0.0019   0.0015   0.0016
LATT  1
SFAC C H B N O P Cl Mo Pt
UNIT 226.00 222.00 4.00 29.00 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 1.134
_oxdiff_exptl_absorpt_empirical_full_min 0.887
_publcif_funding_html
;
;