Construction of an iminoketenylidene.
Burt, Liam K.; Hill, Anthony F.; Chemical communications (Cambridge, England) 57 (2021) 8480–8483; doi:10.1039/d1cc03310g

data_7128665
_publ_section_title
;
 Construction of an iminoketenylidene.
;
_journal_issue                   68
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8480
_journal_page_last               8483
_journal_paper_doi               10.1039/d1cc03310g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C63 H61 B N7 O2 P2 Pt W, 2(C H Cl3), C24 H20 B'
_chemical_formula_sum            'C89 H83 B2 Cl6 N7 O2 P2 Pt W'
_chemical_formula_weight         1957.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-21 deposited with the CCDC.	2021-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.436(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9875(3)
_cell_length_b                   15.7357(2)
_cell_length_c                   26.1799(5)
_cell_measurement_reflns_used    10377
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.7610
_cell_measurement_theta_min      5.0980
_cell_volume                     8334.1(2)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.963
_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  50.00   1.00   17.00    --   36.18 -19.00-120.00   82
  2  \w     15.00  75.00   1.00   17.00    --   36.18 -99.00 -30.00   60
  3  \w    -25.00  55.00   1.00   17.00    --   36.18 -38.00   0.00   80
  4  \w     24.00  51.00   1.00   17.00    --   36.18  57.00-180.00   27
  5  \w     56.00  96.00   1.00   17.00    --   36.18  57.00-180.00   40
  6  \w     93.00 176.00   1.00   68.00    --  109.99  45.00 -30.00   83
  7  \w     44.00 131.00   1.00   68.00    --  109.99 -30.00 -90.00   87
  8  \w     71.00 106.00   1.00   68.00    --  109.99 -95.00-120.00   35
  9  \w     41.00 104.00   1.00   68.00    --  109.99 -95.00 150.00   63
 10  \w     40.00 131.00   1.00   68.00    --  109.99 -30.00   0.00   91
 11  \w     42.00 136.00   1.00   68.00    --  109.99 -77.00   0.00   94
;
_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      0.0757236000
_diffrn_orient_matrix_UB_12      -0.0060958000
_diffrn_orient_matrix_UB_13      0.0213048000
_diffrn_orient_matrix_UB_21      -0.0060565000
_diffrn_orient_matrix_UB_22      0.0125224000
_diffrn_orient_matrix_UB_23      0.0569189000
_diffrn_orient_matrix_UB_31      -0.0056058000
_diffrn_orient_matrix_UB_32      -0.0968203000
_diffrn_orient_matrix_UB_33      0.0060039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28213
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.197
_diffrn_reflns_theta_min         4.216
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.152
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.558
_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 red'
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       plate
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.028
_refine_diff_density_max         2.060
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         16087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0588P)^2^+19.0832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12305
_reflns_number_total             16087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03310g2.cif
_cod_data_source_block           lb043_faces
_cod_depositor_comments
'Adding full bibliography for 7128663--7128667.cif.'
_cod_database_code               7128665
_publcif_datablock.id            {340c82c0-2146-4a79-b0e5-bcc1da740058}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C90H86B2Cl6N7O2P2PtW
_chemical_oxdiff_usercomment     'CHCl3/n-hex vap diff, r.t.'
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 Ternary CH refined with riding coordinates:
 C130(H130), C131(H131)
2.b Aromatic/amide H refined with riding coordinates:
 C55(H55), C15(H15), C41(H41), C65(H65), C35(H35), C61(H61), C42(H42),
 C74(H74), C64(H64), C45(H45), C71(H71), C101(H101), C20(H20), C81(H81),
 C25(H25), C62(H62), C44(H44), C43(H43), C31(H31), C51(H51), C34(H34), C52(H52),
  C95(H95), C01T(H01T), C54(H54), C125(H125), C111(H111), C33(H33), C113(H113),
 C121(H121), C32(H32), C73(H73), C63(H63), C93(H93), C112(H112), C72(H72),
 C102(H102), C91(H91), C85(H85), C105(H105), C53(H53), C115(H115), C103(H103),
 C82(H82), C94(H94), C114(H114), C104(H104), C124(H124), C84(H84), C92(H92),
 C122(H122), C83(H83), C123(H123), C6(H6), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C23(H23A,H23B,
 H23C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C), C10(H10A,H10B,H10C), C5(H5A,
 H5B,H5C)
;
_ins_header
;
TITL LB043_faces in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  20.987531  15.735725  26.179858  90.0000 105.4363  90.0000
ZERR    4.00   0.000310   0.000215   0.000465   0.0000   0.0017   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O P Cl W Pt
UNIT 360.00 344.00 8.00 28.00 8.00 8.00 24.00 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 1.437
_oxdiff_exptl_absorpt_empirical_full_min 0.733
_publcif_funding_html
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;