Protic Ruthenium Tris(pyrazol-3-ylmethyl)amine Complexes Featuring a Hydrogen-Bonding Network in the Second Coordination Sphere.
Yamagishi, Hiroaki; Nabeya, Shohei; Ikariya, Takao; Kuwata, Shigeki; Inorganic chemistry 54 (2015) 11584–11586; doi:10.1021/acs.inorgchem.5b02044

data_4346738
_publ_section_title
;
 Protic Ruthenium Tris(pyrazol-3-ylmethyl)amine Complexes Featuring a
 Hydrogen-Bonding Network in the Second Coordination Sphere.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11584
_journal_page_last               11586
_journal_paper_doi               10.1021/acs.inorgchem.5b02044
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C57 H60 Cl N7 P Ru, Cl'
_chemical_formula_sum            'C57 H60 Cl2 N7 P Ru'
_chemical_formula_weight         1046.10
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 114.5540(18)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.674(3)
_cell_length_b                   23.254(4)
_cell_length_c                   16.722(3)
_cell_measurement_reflns_used    16463
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.03
_cell_volume                     5190.0(17)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0507
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42387
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2176.00
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.310
_refine_diff_density_max         1.610
_refine_diff_density_min         -0.715
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     673
_refine_ls_number_reflns         11692
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 1.3500\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                9531
_reflns_number_total             11692
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5b02044_si_002.cif
_cod_data_source_block           compound3_(RuCl(LH3)(PPh3))Cl
_cod_original_cell_volume        5190.3(16)
_cod_database_code               4346738