Redetermination of tris(ethyl carbazate-κ^2^<i>N</i>,<i>O</i>)cobalt(II) dinitrate
Srinivasan, Krishnan; Govindarajan, Subbaiah; Harrison, William T. A.; Acta Crystallographica Section E 63 (2007) m3028–m3029; doi:10.1107/S1600536807055584

data_2216817
_publ_section_title
;
 Redetermination of tris(ethyl
 carbazate-\k^2^<i>N</i>,<i>O</i>)cobalt(II) dinitrate
;
_journal_coeditor_code           TK2213
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3028
_journal_page_last               m3029
_journal_paper_doi               10.1107/S1600536807055584
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Co (C3 H8 N2 O2)3] (N O3)2'
_chemical_formula_moiety         'C9 H24 Co N6 O6 , 2N O3'
_chemical_formula_sum            'C9 H24 Co N8 O12'
_chemical_formula_weight         495.29
_chemical_name_systematic
;
tris(ethyl carbazate-\k^2^N,O)cobalt(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
_cell_angle_beta                 110.2445(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   28.0291(6)
_cell_length_b                   8.6245(2)
_cell_length_c                   35.6763(7)
_cell_measurement_reflns_used    19276
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     8091.5(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      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f'
_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  0.049
_diffrn_reflns_av_sigmaI/netI    0.042
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            86674
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.9
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         18519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0347P)^2^+4.8866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                14049
_reflns_number_total             18519
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2213.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2216817
_cod_database_fobs_code          2216817