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_4346739
_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         'C45 H52 Cl N8 Ru, Cl, 0.5(C4 H10 O)'
_chemical_formula_sum            'C47 H57 Cl2 N8 O0.5 Ru'
_chemical_formula_weight         914.00
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                101.618(4)
_cell_angle_beta                 93.014(4)
_cell_angle_gamma                90.679(4)
_cell_formula_units_Z            2
_cell_length_a                   9.924(3)
_cell_length_b                   10.888(3)
_cell_length_c                   21.297(5)
_cell_measurement_reflns_used    7839
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.03
_cell_volume                     2250.3(11)
_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 0.956
_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  0.0309
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18402
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             954.00
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.080
_refine_diff_density_max         4.410
_refine_diff_density_min         -1.610
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     575
_refine_ls_number_reflns         9875
_refine_ls_number_restraints     7
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0019Fo^2^ + 2.9900\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                7956
_reflns_number_total             9875
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5b02044_si_002.cif
_cod_data_source_block           compound5_(RuCl(PhNH2)(LH3))Cl.0.5Et2O
_cod_original_cell_volume        2250.2(9)
_cod_original_formula_sum        'C47 H57 Cl2 N8 O0.50 Ru'
_cod_database_code               4346739