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_7710828
_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 N6 O2 P2 Pt0.97 W0.97), 0.06(Pt W), 2(C2 H3 N)'
_chemical_formula_sum            'C112 H110 B2 Cl2 N14 O4 P4 Pt2 W2'
_chemical_formula_weight         2690.41
_chemical_properties_physical    Moisture-sensitive,Heat-sensitive
_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 1.5-alpha
(compiled 2021.04.28 svn.r794ee209 for OlexSys, GUI svn.r6317)
;
_audit_update_record
;
2022-05-15 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                71.013(2)
_cell_angle_beta                 80.492(2)
_cell_angle_gamma                78.1020(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5580(2)
_cell_length_b                   21.0234(3)
_cell_length_c                   24.0391(5)
_cell_measurement_reflns_used    27032
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6490
_cell_measurement_theta_min      3.8850
_cell_volume                     5374.29(18)
_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      150.01(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 0.993
_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      3.00  29.00   1.00    2.48    --   37.29  90.00 -34.44   26
  2  \w     18.00 106.00   1.00    2.48    --   37.29  38.00  30.00   88
  3  \w     18.00 106.00   1.00    2.48    --   37.29  38.00-180.00   88
  4  \w      4.00  30.00   1.00    2.48    --   37.29  88.00 177.27   26
  5  \w      8.00  42.00   1.00    2.48    --   37.29  81.00 -93.63   34
  6  \w     13.00 104.00   1.00    2.48    --   37.29  72.00-138.26   91
  7  \w    -32.00  56.00   1.00    2.48    --   37.29 -38.00-150.00   88
  8  \w      8.00 109.00   1.00    2.48    --   37.29  19.00   0.00  101
  9  \w     27.00  91.00   1.00    2.48    --   37.29-125.00  90.00   64
 10  \w     21.00 105.00   1.00    2.48    --   37.29  57.00  90.00   84
 11  \w     41.00 136.00   1.00    9.91    --  111.00 -25.00 150.00   95
 12  \w    103.00 178.00   1.00    9.91    --  111.00  77.00 -60.00   75
 13  \w     44.00 131.00   1.00    9.91    --  111.00 -64.00 -60.00   87
 14  \w     41.00 109.00   1.00    9.91    --  111.00-111.00 -30.00   68
 15  \w     42.00 130.00   1.00    9.91    --  111.00 -38.00-180.00   88
 16  \w     41.00 109.00   1.00    9.91    --  111.00-111.00-180.00   68
 17  \w     91.00 178.00   1.00    9.91    --  111.00  64.00-180.00   87
 18  \w     41.00 136.00   1.00    9.91    --  111.00 -25.00   0.00   95
 19  \w     41.00 109.00   1.00    9.91    --  111.00-111.00-120.00   68
 20  \w     41.00 109.00   1.00    9.91    --  111.00-111.00 120.00   68
 21  \w     41.00 109.00   1.00    9.91    --  111.00-111.00  30.00   68
 22  \w     44.00 131.00   1.00    9.91    --  111.00 -64.00  90.00   87
 23  \w     41.00 136.00   1.00    9.91    --  111.00 -25.00-120.00   95
 24  \w     43.00 138.00   1.00    9.91    --  111.00 -77.00-120.00   95
 25  \w     41.00 109.00   1.00    9.91    --  111.00-111.00  90.00   68
 26  \w     42.00 178.00   1.00    9.91    --  111.00   0.00 -60.00  136
 27  \w    -64.00  30.00   1.00    2.48    --  -37.29  77.00   0.00   94
 28  \w      4.00  30.00   1.00    2.48    --   37.29  88.00  52.19   26
 29  \w     27.00  91.00   1.00    2.48    --   37.29-125.00 -90.00   64
 30  \w      4.00  30.00   1.00    2.48    --   37.29  88.00 123.91   26
 31  \w    -21.00  64.00   1.00    2.48    --   37.29 -77.00 -60.00   85
 32  \w      4.00  30.00   1.00    2.48    --   37.29  88.00  25.28   26
 33  \w    -32.00  56.00   1.00    2.48    --   37.29 -38.00  60.00   88
 34  \w    -30.00  54.00   1.00    2.48    --   37.29 -57.00   0.00   84
 35  \w      6.00  76.00   1.00    2.48    --   37.29 -99.00-180.00   70
;
_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      -0.1349722000
_diffrn_orient_matrix_UB_12      0.0031598000
_diffrn_orient_matrix_UB_13      0.0174636000
_diffrn_orient_matrix_UB_21      0.0152838000
_diffrn_orient_matrix_UB_22      -0.0780973000
_diffrn_orient_matrix_UB_23      0.0149785000
_diffrn_orient_matrix_UB_31      0.0177421000
_diffrn_orient_matrix_UB_32      -0.0078156000
_diffrn_orient_matrix_UB_33      0.0641567000
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.129
_diffrn_reflns_theta_min         3.880
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.095
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.496
_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 red'
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, MeCN'
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.047
_refine_diff_density_max         3.114
_refine_diff_density_min         -2.017
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1357
_refine_ls_number_reflns         21031
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0233P)^2^+39.0675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18930
_reflns_number_total             21031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01558g2.cif
_cod_data_source_block           lb052_faces
_cod_database_code               7710828
_publcif_datablock.id            {85e3c5fe-faa5-42ba-83fa-1e16079fef66}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C111H108.5B2Cl2N13.5O4P4Pt2W2
_chemical_oxdiff_usercomment     'Vap Diff. THF/MeCN. r.t.'
_reflns_odcompleteness_completeness 99.35
_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
 C2B, O1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C2, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2B \\sim O1B: within 1.16A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.16A
N3 \\sim C2 \\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
4. Others
 Fixed Sof: Pt1B(0.97) W1B(0.97) Pt1C(0.03) W1C(0.03) Pt1D(0.03) W2D(0.03)
 Pt1A(0.97) W1A(0.97) N8(0.5) C73(0.5) H73C(0.5) H73D(0.5) H73E(0.5) C74(0.5)
 C2(0.5) N3(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
5.a Ternary CH refined with riding coordinates:
 B1B(H1B), B1A(H1A)
5.b Aromatic/amide H refined with riding coordinates:
 C6B(H6B), C11B(H11B), C16B(H16B), C21B(H21B), C22B(H22B), C23B(H23B),
 C24B(H24B), C25B(H25B), C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B),
 C35B(H35B), C41B(H41B), C42B(H42B), C43B(H43B), C44B(H44B), C45B(H45B),
 C51B(H51B), C52B(H52B), C53B(H53B), C54B(H54B), C55B(H55B), C61B(H61B),
 C62B(H62B), C63B(H63B), C64B(H64B), C65B(H65B), C71B(H71B), C72B(H72B),
 C73B(H73B), C74B(H74B), C75B(H75B), C6A(H6A), C11A(H11A), C16A(H16A),
 C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C31A(H31A),
 C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C41A(H41A), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A), C51A(H51A), C52A(H52A), C53A(H53A),
 C54A(H54A), C55A(H55A), C61A(H61A), C62A(H62A), C63A(H63A), C64A(H64A),
 C65A(H65A), C71A(H71A), C72A(H72A), C73A(H73A), C74A(H74A), C75A(H75A)
5.c Idealised Me refined as rotating group:
 C4B(H4BA,H4BB,H4BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C13B(H13A,H13B,
 H13C), C14B(H14A,H14B,H14C), C18B(H18A,H18B,H18C), C4A(H4AA,H4AB,H4AC),
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C13A(H13D,H13E,H13F), C14A(H14D,H14E,
 H14F), C18A(H18D,H18E,H18F), C71(H71C,H71D,H71E), C73(H73C,H73D,H73E), C7(H7A,
 H7B,H7C)
;
_shelx_res_checksum              49227
_ins_header
;
TITL LB052_faces in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  11.557974  21.023448  24.039096  71.0128  80.4924  78.1019
ZERR    2.00   0.000229   0.000288   0.000489   0.0015   0.0017   0.0014
LATT  1
SFAC C H B N O P Cl W Pt
UNIT 222.00 217.00 4.00 27.00 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 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.745
_publcif_funding_html
;
;