Cyclometallated ruthenium(ii) complexes with ditopic thienyl‒NHC ligands: syntheses and alkyne annulations
Xie, Xiaoke; Huynh, Han Vinh; Organic Chemistry Frontiers 2 (2015) 1598–; doi:10.1039/C5QO00292C

data_1553192
_publ_section_title
;
 Cyclometallated ruthenium(ii) complexes with ditopic thienyl--NHC
 ligands: syntheses and alkyne annulations
;
_journal_issue                   12
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1598
_journal_paper_doi               10.1039/C5QO00292C
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C30 H29 Cl N2 Ru S'
_chemical_formula_sum            'C30 H29 Cl N2 Ru S'
_chemical_formula_weight         586.13
_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   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-09-16 deposited with the CCDC.
2015-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.422(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4555(4)
_cell_length_b                   15.1572(5)
_cell_length_c                   16.4668(6)
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_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      43.54
_cell_measurement_theta_min      2.39
_cell_volume                     2601.83(16)
_computing_cell_refinement
'SHELXTL, Acta Cryst., Sect. A 2008, 64, 112-122.'
_computing_data_collection       'APEX v2014.9.0'
_computing_data_reduction        'Saint, APEX v2014.9.0.'
_computing_molecular_graphics    Ortep3
_computing_publication_material  'APEX v2014.9.0.'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'Sir 2014'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker AXS D8 Venture '
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36821
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_min         2.371
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         9794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+3.2841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8528
_reflns_number_total             9794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qo00292c2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1553192
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.920
_shelxl_version_number           2014/6
_shelx_res_checksum              12672
_shelx_hkl_checksum              30243