Bis(diethylenetriamine-κ^3^<i>N</i>)nickel(II) 5-amino-1,3,4-thiadiazole-2-sulfonamidate chloride monohydrate
Liu-Gonzalez, M.; Sanz-Ruiz, F.; Chufán, Eduardo E.; Pedregosa, Jose C.; Borras-Tortonda, Joaquin; Acta Crystallographica Section C 57 (2001) 1132–1134; doi:10.1107/S0108270101009088

data_2012275
_publ_section_title
;
 Bis(diethylenetriamine-\k^3^<i>N</i>)nickel(II)
 5-amino-1,3,4-thiadiazole-2-sulfonamidate chloride monohydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1132
_journal_page_last               1134
_journal_paper_doi               10.1107/S0108270101009088
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Ni(C4 H13 N3 )2 ](C2 H3 N4 O2 S2 )Cl , H2 O'
_chemical_formula_moiety
'C8 H26 N6 Ni 2+ , C2 H3 N4 O2 S2 -  , Cl - , H2 O'
_chemical_formula_sum            'C10 H31 Cl N10 Ni O3 S2'
_chemical_formula_weight         497.73
_chemical_name_systematic
;
Bis(diethylenetriamine)nickel(II) 5-amino-1,3,4-thiadiazole-2-
sulfonamidate chloride hydrate.
;
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00(6)
_cell_angle_beta                 99.44(5)
_cell_angle_gamma                90.00(7)
_cell_formula_units_Z            4
_cell_length_a                   8.378(6)
_cell_length_b                   11.099(10)
_cell_length_c                   23.042(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      1.79
_cell_volume                     2114(3)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1997)'
_computing_data_reduction        'Process in Omolen (Nonius, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .944
_diffrn_measured_fraction_theta_max .944
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius Cad-4 difractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_sigmaI/netI    .0486
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            3706
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        .0465
_diffrn_standards_interval_count 1000
_diffrn_standards_interval_time  4500
_diffrn_standards_number         60
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  .880
_exptl_absorpt_correction_T_min  .774
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .10
_refine_diff_density_max         .668
_refine_diff_density_min         -.497
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          .0885
_refine_ls_R_factor_gt           .0594
_refine_ls_shift/su_max          .042
_refine_ls_shift/su_mean         .003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+4.4405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1486
_reflns_number_gt                2685
_reflns_number_total             3706
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1492.cif
_cod_data_source_block           I
_cod_depositor_comments
;
Automatic conversion scripts had previously changed 
'_atom_site_refinement_flags' tag values 'd' into 'D' as recommended by 
'cif_core.dic' version 2.4.1. However, manual inspection revealed that the 
underlying problem was actually related to a wrong tag names inside the 
atom site loop. The following changes were performed to resolve the problem: 

* '_atom_site_refinement_flags' tag was changed to '_atom_site_calc_flag'
* '_atom_site_calc_flag' tag was changed to '_atom_site_site_symmetry_order'
* '_atom_site_disorder_group' tag was changed to 
  '_atom_site_refinement_flags_posn'

Antanas Vaitkus,
2015-03-19

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2012275
_cod_database_fobs_code          2012275