Investigation of nitro–nitrito photoisomerization: crystal structures of <i>trans</i>-{2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}(pyridine/4-methylpyridine)nitrocobalt(III)
Ohba, Shigeru; Tsuchimoto, Masanobu; Yamada, Naoki; Acta Crystallographica Section E 74 (2018) 1759–1763; doi:10.1107/S2056989018015487

data_2242728
_publ_section_title
;
 Investigation of nitro--nitrito photoisomerization: crystal structures of
 <i>trans</i>-{2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}(pyridine/4-methylpyridine)nitrocobalt(III)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1759
_journal_page_last               1763
_journal_paper_doi               10.1107/S2056989018015487
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Co (C16 H14 N2 O2) (N O2) (C5 H5 N)]'
_chemical_formula_moiety         'C21 H19 Co N4 O4'
_chemical_formula_structural     '(Co (C16 H14 N2 O2) (N O2) (C5 H5 N))'
_chemical_formula_sum            'C21 H19 Co N4 O4'
_chemical_formula_weight         450.33
_chemical_name_systematic
<i>trans</i>-{2,2'-[Ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}(nitro-\k<i>N</i>)(pyridine-\k<i>N</i>)cobalt(III)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.924(2)
_cell_length_b                   14.007(3)
_cell_length_c                   40.339(8)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    302
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.50
_cell_volume                     3912.3(16)
_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      302
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            52512
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.771
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.378
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2597 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+1.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                6955
_reflns_number_total             9036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7784sup1.cif
_cod_data_source_block           I
_cod_database_code               2242728
_cod_database_fobs_code          2242728
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.964
_shelx_hkl_checksum              93626
_shelx_res_checksum              97417