Synthesis and structure determination of racemic (Δ/Λ)-tris(ethylenediamine)cobalt(III) trichloride hemi(hexaaquasodium chloride)
Conrad-Marut, Linden H.; Reinheimer, Eric W.; Johnson, Adam R.; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021009336

data_2243918
_publ_section_title
;
 Synthesis and structure determination of racemic
 (\D/\L)-tris(ethylenediamine)cobalt(III) trichloride hemi(hexaaquasodium
 chloride)
;
_journal_coeditor_code           HB7980
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021009336
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Co (C2 H8 N2)3]2 Cl6, [Na (H2 O1)6]Cl'
_chemical_formula_moiety         '2(C6 H24 Co N6), 7(Cl), H12 Na O6'
_chemical_formula_sum            'C12 H60 Cl7 Co2 N12 Na O6'
_chemical_formula_weight         857.72
_chemical_name_systematic
;
(\D/\L)-Tris(ethylenediamine)cobalt(III) trichloride
hemi(hexaaquasodium chloride)
;
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   11.4290(2)
_cell_length_b                   11.4290(2)
_cell_length_c                   15.5815(2)
_cell_measurement_reflns_used    30262
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6570
_cell_measurement_theta_min      2.0590
_cell_volume                     1762.61(5)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_reduction
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CrysAlisPro (Rigaku OD, 2020)
;
_computing_molecular_graphics
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<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
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<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
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ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0086
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65362
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_diffrn_reflns_theta_min         2.614
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_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.664
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_exptl_absorpt_process_details
;
(CrysalisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.217
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_refine_diff_density_min         -0.762
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         1860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0373P)^2^+0.9272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                1643
_reflns_number_total             1860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7980sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2023-01-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         428.86
_cod_original_formula_moiety         'C6 H24 Co1 N6, 3.5(Cl), 0.5(H12 Na1 O6)'
_cod_original_formula_iupac        '[Co (C2 H8 N2)3] Cl3, {[Na (H2 O1)6]Cl}0.5'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        1762.61(7)
_cod_original_formula_sum        'C6 H30 Cl3.50 Co N6 Na0.50 O3'
_cod_database_code               2243918
_cod_database_fobs_code 2243918