Synthesis of Various Cationic Ruthenium-Aqua Complexes with Hydrotris(3,5-diisopropylpyrazolyl)borate Ligand, TpiPrRu(OH2)n(L)3-n.(CF3SO3)(THF)x, and Their Structures Supported by Hydrogen-Bonding Networks1
Yoshiaki Takahashi; Munetaka Akita; Shiro Hikichi; Yoshihiko Moro-oka; Inorganic Chemistry 37 (1998) 3186–3194; doi:10.1021/ic9801802

data_4322871
_publ_contact_author
;
 Munetaka AKITA
 Research Laboratory of Resources Utilization, Tokyo Institute of 
Technology, 4259 Nagatsuta, Midori-ku, Yokohama 227-8503, Japan
;
_publ_contact_author_email       makita@res.titech.ac.jp
_publ_contact_author_fax         +81-45-924-5226
_publ_section_title
;
 Synthesis of Various Cationic Ruthenium-Aqua Complexes with
 Hydrotris(3,5-diisopropylpyrazolyl)borate Ligand,
 TpiPrRu(OH2)n(L)3-n.(CF3SO3)(THF)x, and Their Structures Supported by
 Hydrogen-Bonding Networks1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3186
_journal_page_last               3194
_journal_paper_doi               10.1021/ic9801802
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C49 H90 B F3 N8 O8 Ru S'
_chemical_formula_weight         1120.23
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      36
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_audit_creation_date             'Tue Mar 10 11:36:05 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.121(5)
_cell_length_b                   21.492(5)
_cell_length_c                   17.156(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     5944(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_orient_matrix_UB_11      -0.05673
_diffrn_orient_matrix_UB_12      -0.00051
_diffrn_orient_matrix_UB_13      0.02365
_diffrn_orient_matrix_UB_21      0.01017
_diffrn_orient_matrix_UB_22      -0.04304
_diffrn_orient_matrix_UB_23      0.02008
_diffrn_orient_matrix_UB_31      0.02295
_diffrn_orient_matrix_UB_32      0.01766
_diffrn_orient_matrix_UB_33      0.04934
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3657
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.03
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_meas      ?
_exptl_crystal_description       unknown
_exptl_crystal_F_000             2384.00
_exptl_crystal_size_max          0.000
_exptl_crystal_size_mid          0.000
_exptl_crystal_size_min          0.000
_refine_diff_density_max         0.85
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.282
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     334
_refine_ls_number_reflns         2584
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0524
_refine_ls_shift/esd_max         0.1920
_refine_ls_shift/esd_mean        0.0200
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0338
_reflns_number_observed          2584
_reflns_number_total             3657
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ic9801802_2.cif
_cod_data_source_block           compound3b[TpiPrRu(OH2)2(pziPr-H)(OTf)(THF)2]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00000|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5943(2)
_cod_original_sg_symbol_H-M      'C m c 21 '
_cod_original_formula_sum        'C49 H90 B F3 N8 O8 S Ru '
_cod_database_code               4322871