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

data_7128666
_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, C H Cl3, F6 P'
_chemical_formula_sum            'C64 H62 B Cl3 F6 N7 O2 P3 Pt W'
_chemical_formula_weight         1664.21
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-25 deposited with the CCDC.	2021-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                100.170(3)
_cell_angle_beta                 103.965(3)
_cell_angle_gamma                107.433(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8143(3)
_cell_length_b                   14.7029(4)
_cell_length_c                   22.6429(8)
_cell_measurement_reflns_used    16282
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.1760
_cell_measurement_theta_min      3.6900
_cell_volume                     3507.6(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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     -5.00  36.00   1.00  165.00    --   18.00  77.00 -60.00   41
  2  \w      3.00  92.00   1.00  165.00    --   18.00  37.00 -60.00   89
  3  \w    -14.00  36.00   1.00  165.00    --   18.00  77.00  30.00   50
  4  \w    -10.00  42.00   1.00  165.00    --   18.00  77.00 150.00   52
  5  \w     40.00  95.00   1.00  165.00    --   18.00 178.00 150.00   55
  6  \w      2.00  29.00   1.00  165.00    --   18.00 -37.00 150.00   27
  7  \w     -1.00  97.00   1.00  165.00    --   18.00  19.00-150.00   98
;
_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      0.0660242000
_diffrn_orient_matrix_UB_12      0.0200734000
_diffrn_orient_matrix_UB_13      0.0080915000
_diffrn_orient_matrix_UB_21      -0.0042778000
_diffrn_orient_matrix_UB_22      -0.0195720000
_diffrn_orient_matrix_UB_23      -0.0317573000
_diffrn_orient_matrix_UB_31      -0.0036683000
_diffrn_orient_matrix_UB_32      0.0443836000
_diffrn_orient_matrix_UB_33      -0.0070086000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41979
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         3.287
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.875
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.508
_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 dark purple'
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.850
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         19658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0330P)^2^+13.4745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15114
_reflns_number_total             19658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03310g2.cif
_cod_data_source_block           lb044_faces
_cod_depositor_comments
'Adding full bibliography for 7128663--7128667.cif.'
_cod_original_cell_volume        3507.58(19)
_cod_database_code               7128666
_publcif_datablock.id            {fccc05d5-6b8a-4fed-8df4-a6b4d146f18d}
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C66H57BCl2F6N7O2PPtW
_chemical_oxdiff_usercomment     'CHCl3/nHex, vap diff over 2 weeks 5 degC'
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.471
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_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:
 C86(H86)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C18(H18), C23(H23), C24(H24), C25(H25), 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), C61(H61), C62(H62),
 C63(H63), C64(H64), C65(H65), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C81(H81), C82(H82), C83(H83), C84(H84), C85(H85)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C27(H27A,
 H27B,H27C)
;
_ins_header
;
TITL LB044_faces in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  11.814328  14.702923  22.642947 100.1703 103.9652 107.4329
ZERR    2.00   0.000316   0.000445   0.000815   0.0029   0.0027   0.0025
LATT  1
SFAC C H B N O F P Cl W Pt
UNIT 132.00 114.00 2.00 14.00 4.00 12.00 2.00 4.00 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 1.084
_oxdiff_exptl_absorpt_empirical_full_min 0.944
_publcif_funding_html
;
;