Synthesis of pyridyl carbyne complexes and their conversion to N-heterocyclic vinylidenes
Hill, Anthony; Frogley, Benjamin; Chemical Communications  (2019) –; doi:10.1039/C9CC07760J

data_7125439
_publ_section_title
;
 Synthesis of pyridyl carbyne complexes and their conversion to
 N-heterocyclic vinylidenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07760J
_journal_year                    2019
_chemical_formula_moiety         'C25 H30 B Cl2 N7 O2 Pt W'
_chemical_formula_sum            'C25 H30 B Cl2 N7 O2 Pt W'
_chemical_formula_weight         921.21
_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   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-09-25 deposited with the CCDC.	2019-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.758(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6485(4)
_cell_length_b                   21.1039(9)
_cell_length_c                   13.1797(5)
_cell_measurement_reflns_used    7406
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.1090
_cell_measurement_theta_min      3.7640
_cell_volume                     2960.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 5.1872
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15169
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.964
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.759
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0262P)^2^+18.9741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5334
_reflns_number_total             6356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07760j2.cif
_cod_data_source_block           Compound_10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7125439
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              15971