Hexaaquahexakis(μ~2~-3,5-diamino-1,2,4-triazole)trinickel(II) trisulfate octadecahydrate
Zhang, Guo-Fang; Zhao, Shu-Min; She, Jiang-Bo; Ng, Seik Weng; Acta Crystallographica Section E 63 (2007) m1517–m1518; doi:10.1107/S160053680702051X

data_2213369
_publ_section_title
;
 Hexaaquahexakis(\m~2~-3,5-diamino-1,2,4-triazole)trinickel(II)
 trisulfate octadecahydrate
;
_journal_coeditor_code           HB2392
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1517
_journal_page_last               m1518
_journal_paper_doi               10.1107/S160053680702051X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni3 (C2 H5 N5)6 (H2 O)6] (S O4)3, 18H2 O'
_chemical_formula_moiety
'[(C2 H5 N5)6 (H2 O)6 Ni3] 6+, 3[S O4] 2-, 18(H2 O)'
_chemical_formula_sum            'C12 H78 N30 Ni3 O36 S3'
_chemical_formula_weight         1491.35
_chemical_name_systematic
;
Hexaaquahexakis(\m~2~-3,5-diamino-1,2,4-triazole)trinickel(II) trisulfate
octadecahydrate
;
_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                   12.664(2)
_cell_length_b                   12.664
_cell_length_c                   63.653(6)
_cell_measurement_reflns_used    7201
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      3.2
_cell_volume                     8840.8(16)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Bruker APEX CCD'
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.012
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -82
_diffrn_reflns_number            24396
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.33
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.35
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1P)^2^+10P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.170
_refine_ls_wR_factor_ref         0.180
_reflns_number_gt                1868
_reflns_number_total             2269
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2392.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        8841(2)
_cod_original_sg_symbol_H-M      'R -3c'
_cod_database_code               2213369
_cod_database_fobs_code          2213369