Isonitrile μ2-Carbido Complexes
Hill, Anthony; Burt, Liam K.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02649C

data_7713928
_publ_section_title
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 Isonitrile \m2-Carbido Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02649C
_journal_year                    2023
_chemical_formula_moiety         'C28 H40 B Br N8 O2 Pt W, C H Cl3, C3 H7'
_chemical_formula_sum            'C32 H48 B Br Cl3 N8 O2 Pt W'
_chemical_formula_weight         1152.79
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2023-03-27 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.020(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2377(2)
_cell_length_b                   32.8680(6)
_cell_length_c                   14.4482(3)
_cell_measurement_reflns_used    54739
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.3740
_cell_measurement_theta_min      2.4160
_cell_volume                     4787.56(16)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_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    -15.00  30.00   0.30    8.00    --  -10.52 -99.00  60.00  150
  2  \w    -17.00  83.20   0.30    8.00    --   10.91  57.00-120.00  334
  3  \w    -22.00  41.00   0.30    8.00    --   10.91  77.00 -30.00  210
  4  \w    -15.00  51.00   0.30    8.00    --   10.91 -99.00   0.00  220
  5  \w    -30.00  90.00   0.30    8.00    --   10.91  19.00-180.00  400
  6  \w    -15.00  51.00   0.30    8.00    --   10.91 -99.00  60.00  220
  7  \w    -43.00  16.10   0.30    8.00    --  -10.52  77.00-120.00  197
  8  \w    -42.00  43.20   0.30    8.00    --   10.91 -77.00 120.00  284
  9  \w    -22.00  41.00   0.30    8.00    --   10.91  77.00  30.00  210
 10  \w    -42.00  43.20   0.30    8.00    --   10.91 -77.00-180.00  284
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0226285000
_diffrn_orient_matrix_UB_12      0.0143343000
_diffrn_orient_matrix_UB_13      0.0359144000
_diffrn_orient_matrix_UB_21      0.0359955000
_diffrn_orient_matrix_UB_22      0.0103117000
_diffrn_orient_matrix_UB_23      -0.0306243000
_diffrn_orient_matrix_UB_31      -0.0560428000
_diffrn_orient_matrix_UB_32      0.0124117000
_diffrn_orient_matrix_UB_33      -0.0160443000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            103836
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.780
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.355
_exptl_absorpt_correction_T_max  0.426
_exptl_absorpt_correction_T_min  0.144
_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 yellow'
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.167
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         12380
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0258P)^2^+43.6279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10737
_reflns_number_total             12380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02649c2.cif
_cod_data_source_block           lb023_adjbeamstop_faces
_cod_database_code               7713928
_publcif_datablock.id            {485de739-7894-43d7-9dd7-e3c0dc722093}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H48BBrCl3N8O2PtW
_chemical_oxdiff_usercomment     'CHCl3/Hex, vapour, 5 degC, '
_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. Restrained distances
 C20-C21A \\sim C20-C21B
 with sigma of 0.02
 C22B-H22D \\sim C23A-H22D
 with sigma of 0.02
 C22B-H22F \\sim C23A-H22F
 with sigma of 0.02
 C22B-H22E \\sim C23A-H22E
 with sigma of 0.02
 C20-C22B \\sim C20-C23A
 with sigma of 0.02
3. Rigid bond restraints
 C20, C21A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C20, C22B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C20, C23A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C20, C22A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C20, C21B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C20, C23B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N7, C20
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C20 \\sim C21A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C20 \\sim C23B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C20 \\sim C22B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C20 \\sim C23A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C20 \\sim C21B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C20 \\sim C22A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
N7 \\sim C20: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(C21A) = Uanis(C22A) = Uanis(C23A)
Uanis(C22B) = Uanis(C21B) = Uanis(C23B)
5. Others
 Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Fixed Sof: Cl1(0.5) Cl2(0.5) Cl3(0.5) C29(0.5) H29(0.5) Cl4(0.5) Cl5(0.5)
 Cl6(0.5) C30(0.5) H30(0.5)
6.a Ternary CH refined with riding coordinates:
 B1(H1), C29(H29), C30(H30)
6.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C16(H16)
6.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), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C21A(H21A,H21B,H21C), C22A(H22A,H22B,H22C),
 C23A(H23A,H23B,H23C), C21B(H21D,H21E,H21F), C22B(H22D,H22E,H22F), C23B(H23D,
 H23E,H23F), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              12566
_ins_header
;
TITL LB023_ADJbeamstop_faces in P2/n 
REM P2/n (#13 in standard setting)
CELL 0.71073  10.237729  32.867986  14.448210  90.0000 100.0196  90.0000
ZERR    5.00   0.000168   0.000587   0.000280   0.0000   0.0017   0.0000
LATT  1
SYMM -x+1/2, y,-z+1/2 
SFAC C H B N O Cl Br W Pt
UNIT 160.00 240.00 5.00 40.00 10.00 15.00 5.00 5.00 5.00
TREF
HKLF 4
END
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_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 1.356
_oxdiff_exptl_absorpt_empirical_full_min 0.851
_publcif_funding_html
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