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

data_7125434
_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
'C41 H48 B3 N13 O4 W2, B F4, 2(C H2 Cl2), H2 O'
_chemical_formula_sum            'C43 H54 B3 Cl4 F4 N13 O5 W2'
_chemical_formula_weight         1450.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-09-25 deposited with the CCDC.	2019-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8519(8)
_cell_length_b                   24.1231(13)
_cell_length_c                   14.0794(7)
_cell_measurement_reflns_used    6098
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.0520
_cell_measurement_theta_min      4.1490
_cell_volume                     5383.9(5)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (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  0.0406
_diffrn_reflns_av_unetI/netI     0.0367
_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       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22428
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93161
_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            green
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       needle
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4868
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0265P)^2^+42.8874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3484
_reflns_number_total             4868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07760j2.cif
_cod_data_source_block           Compound_5
_cod_database_code               7125434
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              63584