Transition metal complexes with pyrazole-based ligands. XIX. Diaquabis(3,5-dimethyl-1<i>H</i>-pyrazole-1-carboxamidine-κ^2^<i>N</i>,<i>N</i>')metal(II) dinitrate, with metal = Co and Ni
Jaćimović, Željko K.; Leovac, Vukadin, M.; Mészáros Szécsényi, Katalin; Howard, Judith A. K.; Radosavljević Evans, Ivana; Acta Crystallographica Section C 60 (2004) m467–m470; doi:10.1107/S0108270104017433

data_2014431
_publ_section_title
;Transition metal complexes with pyrazole-based ligands. XIX.
 Diaquabis(3,5-dimethyl-1<i>H</i>-pyrazole-1-carboxamidine-\k^2^<i>N</i>,<i>N</i>')metal(II)
 dinitrate, with metal = Co and Ni
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m467
_journal_page_last               m470
_journal_paper_doi               10.1107/S0108270104017433
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (C6 H10 N4)2 (H2 O)2] (N O3)2'
_chemical_formula_moiety         'C12 H24 Ni N8 O2 2+ , 2N O3 -'
_chemical_formula_sum            'C12 H24 N10 Ni O8'
_chemical_formula_weight         495.10
_chemical_name_systematic
;
Diaquabis(3,5-dimethylpyrazole-1-carboxamidine-\k^2^N,N')nickel(II) dinitrate
;
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 107.251(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.077(3)
_cell_length_b                   10.866(4)
_cell_length_c                   10.456(3)
_cell_measurement_reflns_used    6757
_cell_measurement_temperature    120
_cell_measurement_theta_max      62.15
_cell_measurement_theta_min      5.24
_cell_volume                     984.9(6)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13257
_diffrn_reflns_theta_full        29.497
_diffrn_reflns_theta_max         31.049
_diffrn_reflns_theta_min         2.615
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.47
_refine_ls_goodness_of_fit_ref   0.9759
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2617
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.000637
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994; Prince, 1982),
[weight] = 1/[A~0~T~0~(x)+A~1~T~1~(x) ... +A~n-1~T~n-1~(x)],
where A~i~ are the Chebychev coefficients listed below and x = F~calc~/F~max~
Method = robust weighting (Prince, 1982),
W = [weight] \\times [1-(\DF/6\sF)^2^]^2^.
A~i~ are: 1.85, 2.44 and 0.676
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0648
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                2617
_reflns_number_total             2990
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1571.cif
_cod_data_source_block           II
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_cell_volume        985.0(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C12 H24 Ni N10 O8'
_cod_database_code               2014431
_cod_database_fobs_code          2014431