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_4346737
_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
'C78 H90 Cl3 N14 Ru2, Cl, 3(C2 H4 Cl2), 3(C4 H10 O), H2 O'
_chemical_formula_sum            'C96 H134 Cl10 N14 O4 Ru2'
_chemical_formula_weight         2104.88
_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                 100.321(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.8893(6)
_cell_length_b                   32.5977(13)
_cell_length_c                   21.8979(13)
_cell_measurement_reflns_used    22221
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.04
_cell_volume                     10456.3(9)
_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    'SIR2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0501
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            107615
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4392.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.320
_refine_diff_density_max         5.580
_refine_diff_density_min         -2.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1178
_refine_ls_number_reflns         23451
_refine_ls_number_restraints     21
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0006Fo^2^ + 0.3400\s(Fo^2^) + 80.0000]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1740
_reflns_number_gt                20429
_reflns_number_total             23451
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5b02044_si_002.cif
_cod_data_source_block
compound2_((RuCl(LH3))2(mu-Cl))Cl.H2O.3C2H4Cl2.3Et2O
_cod_database_code               4346737