Investigation of solid-state photochemical nitro‒nitrito linkage isomerization: crystal structures of <i>trans</i>-bis(ethylenediamine)(isothiocyanato)nitritocobalt(III) salts: thiocyanate, chloride monohydrate, and perchlorate‒thiocyanate(0.75/0.25)
Ohba, Shigeru; Tsuchimoto, Masanobu; Kurachi, Saeko; Acta Crystallographica Section E 74 (2018) 1526–1531; doi:10.1107/S2056989018013634

data_2242661
_publ_section_title
;
 Investigation of solid-state photochemical nitro--nitrito linkage
 isomerization: crystal structures of
 <i>trans</i>-bis(ethylenediamine)(isothiocyanato)nitritocobalt(III)
 salts: thiocyanate, chloride monohydrate, and
 perchlorate--thiocyanate(0.75/0.25)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1526
_journal_page_last               1531
_journal_paper_doi               10.1107/S2056989018013634
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Co (C N S) (N O2) (C2 H8 N2)2] (C N S)'
_chemical_formula_moiety         'C5 H16 Co N6 O2 S +, C N S -'
_chemical_formula_structural     '[Co (N O2) (C N S) (C2 H8 N2)2]  (C N S)'
_chemical_formula_sum            'C6 H16 Co N7 O2 S2'
_chemical_formula_weight         341.31
_chemical_name_systematic
;
<i>trans</i>-Bis(ethylenediamine)(isothiocyanato)nitritocobalt(III)
thiocyanate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.2599(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3222(7)
_cell_length_b                   16.0137(6)
_cell_length_c                   11.1284(4)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    299
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.54
_cell_volume                     2728.77(19)
_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      299
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.969
_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  0.0229
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14627
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.911
_diffrn_reflns_theta_min         2.323
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  0.74299
_exptl_absorpt_correction_T_min  0.66703
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_meas      1.65(2)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.917
_refine_ls_extinction_coef       0.0080(10)
_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   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3166
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+7.7542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1730
_reflns_number_gt                2845
_reflns_number_total             3166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7774sup1.cif
_cod_data_source_block           I
_cod_database_code               2242661
_shelx_estimated_absorpt_t_min   0.695
_shelx_estimated_absorpt_t_max   0.744
_shelx_hkl_checksum              1386
_shelx_res_checksum              36106
_cod_database_fobs_code 2242661