Tris(ethyl carbazate-κ^2^<i>N</i>,<i>O</i>)nickel(II) dinitrate
Srinivasan, Krishnan; Govindarajan, Subbaiah; Harrison, William T. A.; Acta Crystallographica Section E 64 (2008) m222–m223; doi:10.1107/S1600536807059053

data_2217281
_publ_section_title
;
 Tris(ethyl carbazate-\k^2^<i>N</i>,<i>O</i>)nickel(II) dinitrate
;
_journal_coeditor_code           SG2208
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m222
_journal_page_last               m223
_journal_paper_doi               10.1107/S1600536807059053
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C3 H8 N2 O2)3] (N O3)2'
_chemical_formula_moiety         'C9 H24 N6 Ni O6 2+ , 2N O3 -'
_chemical_formula_sum            'C9 H24 N8 Ni O12'
_chemical_formula_weight         495.07
_chemical_name_systematic
;
Tris(ethyl carbazate-\k^2^N,<i>O</i>)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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.6520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.0580(8)
_cell_length_b                   8.6571(3)
_cell_length_c                   33.6639(18)
_cell_measurement_reflns_used    6204
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      4.33
_cell_volume                     4092.6(3)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
HKL DENZO (Otwinowski & Minor 1997), HKL SCALEPACK (Otwinowski & Minor
1997)
and SORTAV (Blessing 1995)
;
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       \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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            26981
_diffrn_reflns_theta_full        30.18
_diffrn_reflns_theta_max         30.18
_diffrn_reflns_theta_min         4.33
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         11856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0554P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                6057
_reflns_number_total             11856
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2208.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2217281
_cod_database_fobs_code          2217281