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_4089229
_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         'C60 H63 Cl N4 P2 Ru, 0.5(C6 H14)'
_chemical_formula_sum            'C63 H70 Cl N4 P2 Ru'
_chemical_formula_weight         1081.74
_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                 100.121(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.6071(18)
_cell_length_b                   34.780(5)
_cell_length_c                   12.5004(17)
_cell_measurement_reflns_used    15044
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     5823.8(14)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38502
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2268.00
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.000
_refine_diff_density_min         -1.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     664
_refine_ls_number_reflns         13105
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 9.8000\s(Fo^2^) + 3.0000]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                10375
_reflns_number_total             13105
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om7b00065_si_002.cif
_cod_data_source_block           compound_2a.0.5hexane
_cod_database_code               4089229