Chloridobis(dimethylglyoximato-κ^2^<i>N</i>,<i>N</i>')(4-methylpyridine-κ<i>N</i>)cobalt(III) hemihydrate
Amutha Selvi, Madhavan; Arun Kumar, Kannan; Dayalan, Arunachalam; Acta Crystallographica Section E 67 (2011) m851–m852; doi:10.1107/S1600536811020162

data_2230751
_publ_section_title
;
 Chloridobis(dimethylglyoximato-\k^2^<i>N</i>,<i>N</i>')(4-methylpyridine-\k<i>N</i>)cobalt(III)
 hemihydrate
;
_journal_coeditor_code           JH2292
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m851
_journal_page_last               m852
_journal_paper_doi               10.1107/S1600536811020162
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co (C4 H7 N2 O2)2 Cl (C6 H7 N)], 0.5H2 O'
_chemical_formula_moiety         'C14 H21 Cl Co N5 O4, 0.5(H2 O1)'
_chemical_formula_sum            'C14 H22 Cl Co N5 O4.5'
_chemical_formula_weight         425.74
_chemical_name_systematic
;
Chloridobis(dimethylglyoximato-\k^2^<i>N</i>,<i>N</i>')(4-methylpyridine-
\k<i>N</i>)cobalt(III) hemihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   8.330(5)
_cell_length_b                   14.365(5)
_cell_length_c                   15.634(5)
_cell_measurement_reflns_used    5528
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.60
_cell_volume                     1870.8(14)
_computing_cell_refinement       'APEX2 and SAINT-Plus (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker, 2008)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10519
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.8112
_exptl_absorpt_correction_T_min  0.7720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.382
_refine_ls_abs_structure_details 'Flack (1983), <b>1983 Friedel pairs</b>'
_refine_ls_abs_structure_Flack   0.014(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4642
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0405P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                4143
_reflns_number_total             4642
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jh2292.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen comments.

 Antanas Vaitkus,
 2017-03-25
;
_cod_original_formula_sum        'C14 H22 Cl Co N5 O4.50'
_cod_database_code               2230751
_cod_database_fobs_code          2230751