Synthesis and Structures of NCN Pincer-Type Ruthenium and Iridium Complexes Bearing Protic Pyrazole Arms
Toda, Tatsuro; Saitoh, Koki; Yoshinari, Akihiro; Ikariya, Takao; Kuwata, Shigeki; Organometallics 36 (2017) 1188–; doi:10.1021/acs.organomet.7b00065

data_4089233
_publ_section_title
;
 Synthesis and Structures of NCN Pincer-Type Ruthenium and Iridium
 Complexes Bearing Protic Pyrazole Arms
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1188
_journal_paper_doi               10.1021/acs.organomet.7b00065
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C19 H25 Cl3 Ir N5, 2(C3 H7 N O)'
_chemical_formula_sum            'C25 H39 Cl3 Ir N7 O2'
_chemical_formula_weight         768.21
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 124.857(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.9330(12)
_cell_length_b                   29.341(3)
_cell_length_c                   9.9152(8)
_cell_measurement_reflns_used    6738
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.16
_cell_volume                     3087.4(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32693
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.630
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.930
_refine_diff_density_min         -1.620
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7032
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0011Fo^2^ + 0.4040\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                5099
_reflns_number_total             7033
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om7b00065_si_002.cif
_cod_data_source_block           '_compound_7.2DMF'
_cod_database_code               4089233