Two nickel complexes stabilized by nitrate counter-ions
Freire, Eleonora; Baggio, Sergio; Muñoz, Juan Carlos; Baggio, Ricardo; Acta Crystallographica Section C 58 (2002) m221–m224; doi:10.1107/S0108270102002834

data_2012615
_publ_section_title
;
 Two nickel complexes stabilized by nitrate counter-ions
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m221
_journal_page_last               m224
_journal_paper_doi               10.1107/S0108270102002834
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Ni1 (C18 H12 N6) (H2 O1)3] (N1 O3)2, 3H2 O1'
_chemical_formula_moiety         'C18 H18 N6 Ni O3 2+, 2N O3 1-, 3H2 O'
_chemical_formula_sum            'C18 H24 N8 Ni O12'
_chemical_formula_weight         603.16
_chemical_name_systematic
;
Triaqua-(2,4,6-tris(2-Pyridyl)-1,3,5-triazine-N,N',N")nickel(II),
dinitrate, trihydrate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 100.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.328(2)
_cell_length_b                   14.851(3)
_cell_length_c                   14.124(3)
_cell_measurement_reflns_used    7432
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.17
_cell_volume                     2546.1(9)
_computing_cell_refinement       'SAINT-NT (Bruker, 2000)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'XP in SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_max 0.712
_diffrn_measurement_device_type  'Bruker CCD 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  0.027
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7312
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   'empirical from intensities'
_exptl_absorpt_process_details   'SADABS in SAINT_NT (Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.304
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.087(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         3955
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.041
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0747P)^2^] where P  = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.092
_reflns_number_gt                3550
_reflns_number_total             3955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk1640.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times).

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

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (6
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2546.0(8)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2012615