Hexaaquahexakis(μ~2~-3,5-diamino-4<i>H</i>-1,2,4-triazole)trinickel(II) tris(hexafluoridosilicate) icosahydrate
Wu, Li-Ping; Zhao, Shu-Ming; Zhang, Guo-Fang; Ng, Seik Weng; Acta Crystallographica Section E 64 (2008) m802–; doi:10.1107/S1600536808013329

data_2218529
_publ_section_title
;
 Hexaaquahexakis(\m~2~-3,5-diamino-4<i>H</i>-1,2,4-triazole)trinickel(II)
 tris(hexafluoridosilicate) icosahydrate
;
_journal_coeditor_code           SI2084
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m802
_journal_paper_doi               10.1107/S1600536808013329
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni3 (C2 H5 N5)6 (H2 O)6] [Si F6]3, 20H2 O'
_chemical_formula_moiety         'C12 H42 N30 Ni3 O6 6+, 3(Si F6 2-), 20 H2 O'
_chemical_formula_sum            'C12 H82 F18 N30 Ni3 O26 Si3'
_chemical_formula_weight         1665.48
_chemical_name_systematic
;
Hexaaquahexakis(\m~2~-3,5-diamino-4H-1,2,4-triazole)trinickel(II)
tris(hexafluoridosilicate) icosahydrate
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.0240(10)
_cell_length_b                   13.024
_cell_length_c                   64.462(5)
_cell_measurement_reflns_used    5839
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      3.1
_cell_volume                     9469.4(10)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0098
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            25347
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2420
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+17.0807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                2093
_reflns_number_total             2420
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2084.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        9469.8(9)
_cod_original_sg_symbol_H-M      'R -3c'
_cod_database_code               2218529
_cod_database_fobs_code          2218529