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_2242662
_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] Cl, H2 O'
_chemical_formula_moiety         'C5 H16 Co N6 O2 S 1+, Cl 1-, H2 O'
_chemical_formula_structural     '[Co (N O2) (C N S) (C2 H8 N2)2] Cl, H2 O'
_chemical_formula_sum            'C5 H18 Cl Co N6 O3 S'
_chemical_formula_weight         336.69
_chemical_name_systematic
;
<i>trans</i>-Bis(ethylenediamine)(isothiocyanato)nitritocobalt(III)
chloride monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.295(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9059(4)
_cell_length_b                   12.3302(5)
_cell_length_c                   12.2915(5)
_cell_measurement_reflns_used    9532
_cell_measurement_temperature    301
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.34
_cell_volume                     1348.67(10)
_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 0.982
_diffrn_measured_fraction_theta_max 0.976
_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  0.0238
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14312
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.916
_diffrn_reflns_theta_min         2.341
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.537
_refine_ls_extinction_coef       0.018(3)
_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   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0994P)^2^+0.7693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                2830
_reflns_number_total             3153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7774sup1.cif
_cod_data_source_block           II
_cod_database_code               2242662
_cod_database_fobs_code          2242662
_shelx_estimated_absorpt_t_min   0.686
_shelx_estimated_absorpt_t_max   0.736
_shelx_hkl_checksum              56726
_shelx_res_checksum              30097