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

data_7125433
_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         'C23 H26 B N7 O2 W, C2 H3 N'
_chemical_formula_sum            'C25 H29 B N8 O2 W'
_chemical_formula_weight         668.22
_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
_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                 96.715(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3086(6)
_cell_length_b                   9.8592(4)
_cell_length_c                   17.7914(7)
_cell_measurement_reflns_used    9051
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.5670
_cell_measurement_theta_min      3.6400
_cell_volume                     2666.85(18)
_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 0.997
_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  0.0600
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14443
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.370
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70386
_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            'dark orange'
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.919
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0455
_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^)+15.8480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4122
_reflns_number_total             4702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07760j2.cif
_cod_data_source_block           Compound_2
_cod_original_cell_volume        2666.84(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7125433
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              85060