Syntheses and Crystal Structures of Ruthenium Complexes of 1,4,8,11-Tetraazacyclotetradecane, Tris(2-aminoethyl)amine (tren), and Bis(2-aminoethyl)(iminomethyl)amine. A Microporous Layered Structure Consisting of {[K(tren)]2[RuCl6]}nn- and {(H5O2)4[RuCl6]}nn+
Ken Sakai; Yasutaka Yamada; Taro Tsubomura; Inorganic Chemistry 35 (1996) 3163–3172; doi:10.1021/ic950688u

data_4323822
_publ_contact_author
;
    Dr Ken Sakai
    Department of Industrial Chemistry
    Faculty of Engineering
    Seikei University
    Kichijoji-Kitamachi 3
    Musashino, Tokyo 180
    Japan
;
_publ_contact_author_email       ksakai@chgw.ch.seikei.ac.jp
_publ_contact_author_fax         +81-422-37-3871
_publ_contact_author_phone       '+81-422-37-3759 '
_publ_section_title
;
 Syntheses and Crystal Structures of Ruthenium Complexes of
 1,4,8,11-Tetraazacyclotetradecane, Tris(2-aminoethyl)amine (tren), and
 Bis(2-aminoethyl)(iminomethyl)amine. A Microporous Layered Structure
 Consisting of {[K(tren)]2[RuCl6]}nn- and {(H5O2)4[RuCl6]}nn+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3163
_journal_page_last               3172
_journal_paper_doi               10.1021/ic950688u
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         '(H5 O2)2, C6 H18 K1, Cl6 Ru1'
_chemical_formula_sum            'C6 H28 Cl6 K N4 O4 Ru'
_chemical_formula_weight         573.20
_chemical_name_systematic
;
bis(diaquahydrogen) tris(2-aminoethyl)aminepotassium hexachlororuthenium(III) 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_date             95-10-16
_audit_creation_method           'teXsan (modified by Ken Sakai)'
_audit_update_record
;
95-10-17    text and data added by Ken Sakai
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6.00
_cell_length_a                   10.254(4)
_cell_length_b                   10.254
_cell_length_c                   35.03(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      34.88
_cell_measurement_theta_min      23.55
_cell_volume                     3189.8(15)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_computing_structure_solution    SAPI91
_diffrn_ambient_temperature      293.0
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \q/2\q
_diffrn_orient_matrix_UB_11      0.03352
_diffrn_orient_matrix_UB_12      0.10961
_diffrn_orient_matrix_UB_13      -0.00197
_diffrn_orient_matrix_UB_21      -0.01046
_diffrn_orient_matrix_UB_22      0.00460
_diffrn_orient_matrix_UB_23      0.02828
_diffrn_orient_matrix_UB_31      0.10699
_diffrn_orient_matrix_UB_32      0.02537
_diffrn_orient_matrix_UB_33      0.00338
_diffrn_radiation_detector       'scintillation,NaI,Rigaku SC-30'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2269
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0.27
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.703
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi-scan (North's method)'
_exptl_crystal_colour            reddish-brown
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       plate
_exptl_crystal_F_000             1734.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.52
_refine_diff_density_min         -1.24
_refine_ls_abs_structure_details
;
none
;
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.54
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    13
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1343
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0504
_refine_ls_shift/esd_max         0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma_w=1/\s^2^(F)
_refine_ls_wR_factor_obs         0.0455
_reflns_number_observed          1343
_reflns_number_total             2080
_reflns_observed_criterion       I_>_3.0_sigma(I)
_cod_data_source_file            ic950688u_3.cif
_cod_data_source_block           complex_4
_cod_original_cell_volume        3190(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C6 Cl6 H28 K1 N4 O4 Ru1'
_cod_database_code               4323822