#------------------------------------------------------------------------------
#$Date: 2023-01-25 10:34:33 +0200 (Wed, 25 Jan 2023) $
#$Revision: 280578 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243918.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243918
loop_
_publ_author_name
'Conrad-Marut, Linden H.'
'Reinheimer, Eric W.'
'Johnson, Adam R.'
_publ_section_title
;
 Synthesis and structure determination of racemic
 (Δ/Λ)-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
;
(Δ/Λ)-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
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
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       'ω 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
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.885
_diffrn_reflns_theta_min         2.614
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   analytical
_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
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.762
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_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/[σ²(Fo²)+(0.0373P)²+0.9272P] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.3333 0.6667 0.88151(2) 0.01756(9) Uani d 1 . .
Cl Cl1 0.10242(4) 0.61265(4) 0.62517(2) 0.03423(11) Uani d 1 . .
Cl Cl2 0.0000 1.0000 0.5000 0.0546(3) Uani d 1 . .
Na Na1 0.0000 1.0000 0.7500 0.0543(5) Uani d 1 . .
N N1 0.29983(13) 0.51120(12) 0.95321(8) 0.0244(2) Uani d 1 . .
N N2 0.18593(13) 0.53380(13) 0.80958(8) 0.0273(2) Uani d 1 . .
O O1 0.08849(18) 0.88917(17) 0.65619(12) 0.0592(4) Uani d 1 . .
H H1E 0.0758 0.9001 0.6015 0.089 Uiso d 1 . .
C C1 0.17218(16) 0.39077(15) 0.92577(10) 0.0302(3) Uani d 1 . .
C C2 0.16421(17) 0.39746(16) 0.82971(10) 0.0316(3) Uani d 1 . .
H H2C 0.235(2) 0.386(2) 0.8014(13) 0.036(5) Uiso d 1 . .
H H1A 0.363(2) 0.494(2) 0.9459(13) 0.036(5) Uiso d 1 . .
H H1C 0.171(2) 0.310(2) 0.9475(15) 0.042(6) Uiso d 1 . .
H H1D 0.103(2) 0.396(2) 0.9513(13) 0.033(5) Uiso d 1 . .
H H2D 0.081(2) 0.332(2) 0.8111(13) 0.040(6) Uiso d 1 . .
H H2A 0.114(2) 0.533(2) 0.8215(14) 0.038(5) Uiso d 1 . .
H H1B 0.291(2) 0.519(2) 1.0044(14) 0.038(5) Uiso d 1 . .
H H2B 0.198(2) 0.546(2) 0.7578(14) 0.042(6) Uiso d 1 . .
H H1F 0.105(4) 0.824(4) 0.639(2) 0.096(11) Uiso d 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -1 5 0.0831
-2 0 -5 0.1171
4 1 5 0.0771
-1 1 -1 0.1528
-5 5 -3 0.1820
3 -5 -5 0.1159
0 0 1 0.1083
0 0 -1 0.1083
5 0 3 0.0883
-5 0 -3 0.1574
2 -5 0 0.1260
-2 5 0 0.2152
0 1 -1 0.1341
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Co1 N1 3_565 2_665 90.94(5) ?
N1 Co1 N1 3_565 . 90.94(5) ?
N1 Co1 N1 2_665 . 90.94(5) ?
N2 Co1 N1 3_565 3_565 85.48(5) ?
N2 Co1 N1 . 2_665 174.50(5) ?
N2 Co1 N1 . . 85.48(5) ?
N2 Co1 N1 . 3_565 93.29(6) ?
N2 Co1 N1 3_565 . 174.50(5) ?
N2 Co1 N1 2_665 3_565 174.50(6) ?
N2 Co1 N1 2_665 . 93.29(6) ?
N2 Co1 N1 3_565 2_665 93.29(6) ?
N2 Co1 N1 2_665 2_665 85.48(5) ?
N2 Co1 N2 3_565 2_665 90.55(6) ?
N2 Co1 N2 3_565 . 90.55(6) ?
N2 Co1 N2 . 2_665 90.55(6) ?
O1 Na1 O1 5_676 4_466 88.27(6) ?
O1 Na1 O1 5_676 . 96.03(8) ?
O1 Na1 O1 . 4_466 174.05(8) ?
O1 Na1 O1 3_465 5_676 174.05(8) ?
O1 Na1 O1 3_465 4_466 87.75(8) ?
O1 Na1 O1 6_556 5_676 88.27(6) ?
O1 Na1 O1 6_556 . 87.75(8) ?
O1 Na1 O1 3_465 2_675 88.27(6) ?
O1 Na1 O1 2_675 . 88.27(6) ?
O1 Na1 O1 6_556 2_675 174.05(8) ?
O1 Na1 O1 6_556 4_466 88.27(6) ?
O1 Na1 O1 5_676 2_675 87.75(9) ?
O1 Na1 O1 3_465 . 88.27(6) ?
O1 Na1 O1 3_465 6_556 96.03(8) ?
O1 Na1 O1 2_675 4_466 96.03(8) ?
Co1 N1 H1A . . 109.1(14) ?
Co1 N1 H1B . . 115.9(15) ?
C1 N1 Co1 . . 109.36(9) ?
C1 N1 H1A . . 108.0(14) ?
C1 N1 H1B . . 105.5(16) ?
H1A N1 H1B . . 109(2) ?
Co1 N2 H2A . . 109.7(15) ?
Co1 N2 H2B . . 115.3(15) ?
C2 N2 Co1 . . 108.69(9) ?
C2 N2 H2A . . 107.2(16) ?
C2 N2 H2B . . 108.5(15) ?
H2A N2 H2B . . 107(2) ?
Na1 O1 H1E . . 111.2 ?
Na1 O1 H1F . . 156(2) ?
H1E O1 H1F . . 87.3 ?
N1 C1 C2 . . 107.24(12) ?
N1 C1 H1C . . 108.8(14) ?
N1 C1 H1D . . 107.4(13) ?
C2 C1 H1C . . 115.0(13) ?
C2 C1 H1D . . 110.8(13) ?
H1C C1 H1D . . 107.4(18) ?
N2 C2 C1 . . 106.33(12) ?
N2 C2 H2C . . 109.2(13) ?
N2 C2 H2D . . 110.3(13) ?
C1 C2 H2C . . 111.2(12) ?
C1 C2 H2D . . 109.8(13) ?
H2C C2 H2D . . 110.0(18) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 N1 3_565 1.9676(12) ?
Co1 N1 2_665 1.9676(12) ?
Co1 N1 . 1.9677(12) ?
Co1 N2 3_565 1.9601(12) ?
Co1 N2 2_665 1.9601(12) ?
Co1 N2 . 1.9600(12) ?
Na1 O1 2_675 2.4586(19) ?
Na1 O1 5_676 2.4586(19) ?
Na1 O1 4_466 2.4587(19) ?
Na1 O1 . 2.4586(19) ?
Na1 O1 3_465 2.4586(19) ?
Na1 O1 6_556 2.4586(19) ?
N1 C1 . 1.4825(19) ?
N1 H1A . 0.84(2) ?
N1 H1B . 0.81(2) ?
N2 C2 . 1.484(2) ?
N2 H2A . 0.84(2) ?
N2 H2B . 0.82(2) ?
O1 H1E . 0.8837 ?
O1 H1F . 0.89(4) ?
C1 C2 . 1.504(2) ?
C1 H1C . 0.97(2) ?
C1 H1D . 0.91(2) ?
C2 H2C . 0.99(2) ?
C2 H2D . 0.92(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A Cl1 5_666 0.84(2) 2.57(2) 3.3586(13) 156.7(18)
N1 H1B Cl1 12_566 0.81(2) 2.75(2) 3.4317(13) 142.0(19)
N2 H2A Cl1 6_556 0.84(2) 2.50(2) 3.3286(14) 172(2)
N2 H2B Cl1 . 0.82(2) 2.62(2) 3.2925(13) 140.6(19)
O1 H1E Cl2 . 0.88 2.35 3.1354(18) 147
O1 H1F Cl1 . 0.89(4) 2.41(4) 3.2787(18) 164(3)
C2 H2D O1 4_456 0.92(2) 2.59(2) 3.361(2) 142.1(17)

_cod_database_fobs_code 2243918
