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

data_7125437
_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
'C42 H50 B2 N13 O4 W2, C F3 O3 S, 2.5(C H Cl3)'
_chemical_formula_sum            'C45.5 H52.5 B2 Cl7.5 F3 N13 O7 S W2'
_chemical_formula_weight         1637.76
_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   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                88.518(3)
_cell_angle_beta                 76.527(3)
_cell_angle_gamma                70.518(3)
_cell_formula_units_Z            4
_cell_length_a                   13.6197(4)
_cell_length_b                   18.3015(8)
_cell_length_c                   26.9010(9)
_cell_measurement_reflns_used    14736
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      70.7350
_cell_measurement_theta_min      4.2730
_cell_volume                     6137.7(4)
_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 8.1297
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34502
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72485
_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            yellow
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       prism
_exptl_crystal_F_000             3204
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.033
_refine_diff_density_max         3.501
_refine_diff_density_min         -2.787
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1487
_refine_ls_number_reflns         21463
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0796P)^2^+47.3258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17107
_reflns_number_total             21463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07760j2.cif
_cod_data_source_block           Compound_7
_cod_original_formula_sum        'C45.50 H52.50 B2 Cl7.50 F3 N13 O7 S W2'
_cod_database_code               7125437
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              92432