Investigation of nitro–nitrito photoisomerization: crystal structures of <i>trans</i>-bis(acetylacetonato-<i>O</i>,<i>O</i>')(pyridine/4-methylpyridine/3-hydroxypridine)nitrocobalt(III)
Ohba, Shigeru; Tsuchimoto, Masanobu; Miyazaki, Hiroki; Acta Crystallographica Section E 74 (2018) 1637–1642; doi:10.1107/S2056989018014731

data_2242690
_publ_section_title
;
 Investigation of nitro--nitrito photoisomerization: crystal structures of
 <i>trans</i>-bis(acetylacetonato-<i>O</i>,<i>O</i>')(pyridine/4-methylpyridine/3-hydroxypridine)nitrocobalt(III)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1637
_journal_page_last               1642
_journal_paper_doi               10.1107/S2056989018014731
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Co (C5 H7 O2)2 (N O2) (C5 H5 N)]'
_chemical_formula_moiety         'C15 H19 Co N2 O6'
_chemical_formula_structural     '(Co (C5 H7 O2)2 (N O2) (C5 H5 N))'
_chemical_formula_sum            'C15 H19 Co N2 O6'
_chemical_formula_weight         382.25
_chemical_name_systematic
<i>trans</i>-Bis(acetylacetonato-\k^2^<i>O</i>,<i>O</i>')(nitro)(pyridine-\k<i>N</i>)cobalt(III)
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.588(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1971(14)
_cell_length_b                   13.942(2)
_cell_length_c                   7.4148(11)
_cell_measurement_reflns_used    2813
_cell_measurement_temperature    301
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.75
_cell_volume                     847.1(2)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008) and CAVITY (Ohashi <i>et al.</i>,
1981)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014  (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      301
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.916
_diffrn_reflns_theta_min         2.748
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.343
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.41(3)
_refine_ls_extinction_coef       0.0076(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1529
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.1288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                1449
_reflns_number_total             1529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7778sup1.cif
_cod_data_source_block           I
_cod_database_code               2242690
_cod_database_fobs_code          2242690
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.876
_shelx_hkl_checksum              91676
_shelx_res_checksum              79216