Tris(3-nitropentane-2,4-dionato-κ^2^<i>O</i>,<i>O</i>')cobalt(III)
Johnston, Dean H.; Brangham, Jack T.; Rapp, Christopher D.; Acta Crystallographica Section E 68 (2012) m312–m313; doi:10.1107/S160053681200668X

data_2234068
_publ_section_title
;
 Tris(3-nitropentane-2,4-dionato-\k^2^<i>O</i>,<i>O</i>')cobalt(III)
;
_journal_coeditor_code           ZL2451
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m312
_journal_page_last               m313
_journal_paper_doi               10.1107/S160053681200668X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Co (C5 H6 N O4)3]'
_chemical_formula_moiety         'C15 H18 Co N3 O12'
_chemical_formula_sum            'C15 H18 Co N3 O12'
_chemical_formula_weight         491.25
_chemical_name_common            tris(3-nitro-acetylacetonato)cobalt(III)
_chemical_name_systematic
;
Tris(3-nitropentane-2,4-dionato-\k^2^<i>O</i>,<i>O</i>')cobalt(III)
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2011.4-1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   32.7078(18)
_cell_length_b                   32.7078(18)
_cell_length_c                   7.4976(6)
_cell_measurement_reflns_used    8816
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.59
_cell_measurement_theta_min      2.49
_cell_volume                     8020.9(9)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'GIS (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
;
PLATON (Spek, 2009), Mercury (Macrae <i>et al.</i>, 2008) and
POV-Ray (Cason,
2004)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) and OLEX2 (Dolomanov <i>et al.</i>,
2009)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            24724
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.7560
_exptl_absorpt_correction_T_min  0.6648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.187
_refine_ls_abs_structure_details 'Flack (1983), 1466 Friedel pairs'
_refine_ls_abs_structure_Flack   0.003(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0316P)^2^+2.8577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                3151
_reflns_number_total             3393
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2451.cif
_cod_data_source_block           I
_cod_database_code               2234068
_cod_database_fobs_code          2234068