Bis[μ-4-amino-3,5-bis(hydroxymethyl)-1,2,4-triazole]bis{bis[4-amino-3,5-bis(hydroxymethyl)-1,2,4-triazole]nickel(II)} tetranitrate methanol disolvate
Yu-Peng Pan; Da-Cheng Li; Da-Qi Wang; Acta Crystallographica Section E 64 (2008) m96–m97; doi:10.1107/S1600536807064148

data_2217157
_publ_section_title
;Bis[\m-4-amino-3,5-bis(hydroxymethyl)-1,2,4-triazole]bis{bis[4-amino-3,5-bis(hydroxymethyl)-1,2,4-triazole]nickel(II)}
 tetranitrate methanol disolvate
;
_journal_coeditor_code           KP2150
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m96
_journal_page_last               m97
_journal_paper_doi               10.1107/S1600536807064148
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni2 (C4 H8 N4 O2)6](N O3)4, 2C H4 O'
_chemical_formula_moiety         'C24 H48 N26 Ni2 O18 2+, 4(N O3 -), 2(C H4 O)'
_chemical_formula_sum            'C26 H56 N28 Ni2 O26'
_chemical_formula_weight         1294.41
_chemical_name_systematic
;
Bis[\m-4-amino-3,5-bis(hydroxymethyl)-1,2,4-triazole]bis{bis[4-amino-3,5-
bis(hydroxymethyl)-1,2,4-triazole]nickel(II)} tetranitrate methanol disolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.699(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5126(17)
_cell_length_b                   13.2808(18)
_cell_length_c                   16.153(2)
_cell_measurement_reflns_used    2129
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.226
_cell_measurement_theta_min      2.525
_cell_volume                     2681.3(6)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0939
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12772
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.9019
_exptl_absorpt_correction_T_min  0.8482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1881
_reflns_number_gt                2751
_reflns_number_total             4719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            kp2150.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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        2681.3(7)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               2217157
_cod_database_fobs_code          2217157