Synthesis and Alkyne Insertion Reactions of NHC-Based Cyclometalated Ruthenium(II) Complexes
Ma, Chong; Ai, Chunjin; Li, Zhefu; Li, Bin; Song, Haibin; Xu, Shansheng; Wang, Baiquan; Organometallics 33 (2014) 5164–; doi:10.1021/om500369g

data_4084724
_publ_section_title
;
 Synthesis and Alkyne Insertion Reactions of NHC-Based Cyclometalated
 Ruthenium(II) Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5164
_journal_paper_doi               10.1021/om500369g
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C29 H32 Br Cl N2 Ru'
_chemical_formula_sum            'C29 H32 Br Cl N2 Ru'
_chemical_formula_weight         624.99
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6170(14)
_cell_length_b                   14.7440(16)
_cell_length_c                   26.168(3)
_cell_measurement_reflns_used    21011
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      34.00
_cell_measurement_theta_min      2.60
_cell_volume                     5253.7(10)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            67884
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.068
_diffrn_reflns_theta_min         2.563
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_refine_diff_density_max         3.777
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.375(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         20122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0391P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                16494
_reflns_number_total             20122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500369g_si_001.cif
_cod_data_source_block           2d
_cod_database_code               4084724
_shelx_estimated_absorpt_t_min   0.594
_shelx_estimated_absorpt_t_max   0.639
_shelxl_version_number           2013-2
_shelx_res_checksum              74784
_shelx_hkl_checksum              57133