Double-salt formation in crystal structures containing [Co(en)<sub>3</sub>]Cl<sub>3</sub>.
Kollitz, Megan R.; Lappin, A. Graham; Oliver, Allen G.; Acta crystallographica. Section C, Structural chemistry 79 (2023) 164–169; doi:10.1107/S2053229623002711

data_2312125
_publ_section_title
;
 Double-salt formation in crystal structures containing
 [Co(en)<sub>3</sub>]Cl<sub>3</sub>.
;
_journal_coeditor_code           ZO3032
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              164
_journal_page_last               169
_journal_paper_doi               10.1107/S2053229623002711
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Co (C2 H8 N2)3] Cl3, 4H2 O'
_chemical_formula_moiety         'C6 H24 Co N6 3+, 3(Cl -), 4(H2 O)'
_chemical_formula_sum            'C6 H32 Cl3 Co N6 O4'
_chemical_formula_weight         417.65
_chemical_name_systematic
;
Bis[tris(ethane-1,2-diamine-\k^2^<i>N</i>,<i>N</i>')cobalt(III)] trichloride
tetrahydrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   11.3193(9)
_cell_length_b                   11.3193(9)
_cell_length_c                   15.4254(16)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.64
_cell_volume                     1711.6(3)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
XP (Bruker, 2015) and Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
CIFTAB (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33152
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         1.320
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.491
_exptl_absorpt_correction_T_max  0.8680
_exptl_absorpt_correction_T_min  0.7840
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       needle
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.843
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1430
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+1.0501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                1347
_reflns_number_total             1430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3032sup1.cif
_cod_data_source_block           Coen3Cl
_cod_database_code               2312125
_shelx_estimated_absorpt_t_min   0.722
_shelx_estimated_absorpt_t_max   0.799
_shelx_hkl_checksum              68039
_shelx_res_checksum              32135
_cod_database_fobs_code 2312125