#------------------------------------------------------------------------------
#$Date: 2022-07-06 10:28:17 +0200 (Wed 06 de Jul de 2022) $
#$Revision: 276663 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/15/7061541.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7061541
loop_
_publ_author_name
'Darii, Mariana'
'Beleaev, Ecaterina S.'
'Kravtsov, Victor Ch.'
'Bourosh, Paulina'
'Chumakov, Yurii'
'Hauser, Jürg'
'Decurtins, Silvio'
'Liu, Shi-Xia'
'Sultanova, Olga'
'Baca, Svetlana G.'
_publ_section_title
;
 Crystalline multicomponent compounds involving hexaammine cobalt(iii)
 cations
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11404
_journal_page_last               11421
_journal_paper_doi               10.1039/D2NJ01655A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_sum            'C16 H34 Cl Co N6 O11'
_chemical_formula_weight         580.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-05-20 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                93.856(5)
_cell_angle_beta                 90.491(3)
_cell_angle_gamma                97.850(3)
_cell_formula_units_Z            2
_cell_length_a                   7.35555(13)
_cell_length_b                   10.3264(6)
_cell_length_c                   16.0130(10)
_cell_measurement_reflns_used    3230
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.0120
_cell_measurement_theta_min      2.7820
_cell_volume                     1201.97(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    MERCURY
_computing_publication_material
;
SHELX-97 (Sheldrick, 2008)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7437
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.996
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         7437
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0408
_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/[σ²(Fo²)+(0.0439P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5362
_reflns_number_total             7437
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2nj01655a2.cif
_cod_data_source_block           14sd081
_cod_depositor_comments
'Adding full bibliography for 7061540--7061548.cif.'
_cod_database_code               7061541
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.965
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.80704(7) 0.22169(4) 0.13111(3) 0.01663(14) Uani 1 1 d . . . . .
Cl1 Cl 0.29415(13) 0.14598(8) 0.00057(6) 0.0244(2) Uani 1 1 d . . . . .
O1 O 0.5595(3) 0.4641(2) 0.29735(16) 0.0289(7) Uani 1 1 d . . . . .
O2 O 0.5568(4) 0.6359(3) 0.22393(17) 0.0345(7) Uani 1 1 d . . . . .
H1O H 0.5824 0.7193 0.2116 0.052 Uiso 1 1 d R U . . .
O3 O 0.7052(4) 0.8585(2) 0.22709(15) 0.0334(7) Uani 1 1 d . . . . .
O4 O 0.8838(4) 1.0000(3) 0.31112(17) 0.0327(7) Uani 1 1 d . . . . .
O5 O 0.0196(4) 0.5302(3) 0.26312(18) 0.0468(9) Uani 1 1 d . . . . .
O6 O 0.0970(4) 0.7042(3) 0.19402(19) 0.0439(8) Uani 1 1 d . . . . .
O7 O 0.2558(4) 0.9217(2) 0.21471(16) 0.0322(7) Uani 1 1 d . . . . .
H2O H 0.2021 0.8442 0.1943 0.048 Uiso 1 1 d R U . . .
O8 O 0.4057(4) 1.0516(2) 0.31313(16) 0.0309(7) Uani 1 1 d . . . . .
N1 N 1.0222(4) 0.3521(3) 0.11749(18) 0.0195(7) Uani 1 1 d . . . . .
H1A H 1.0176 0.4224 0.1544 0.029 Uiso 1 1 calc R U . . .
H1B H 1.0231 0.3783 0.0643 0.029 Uiso 1 1 calc R U . . .
H1C H 1.1259 0.3162 0.1274 0.029 Uiso 1 1 calc R U . . .
N2 N 0.8350(4) 0.2568(3) 0.25306(17) 0.0204(7) Uani 1 1 d . . . . .
H2A H 0.7620 0.3172 0.2707 0.031 Uiso 1 1 calc R U . . .
H2B H 0.9541 0.2881 0.2663 0.031 Uiso 1 1 calc R U . . .
H2C H 0.8017 0.1812 0.2786 0.031 Uiso 1 1 calc R U . . .
N3 N 0.5905(4) 0.0929(3) 0.14580(18) 0.0192(7) Uani 1 1 d . . . . .
H3A H 0.5465 0.1056 0.1982 0.029 Uiso 1 1 calc R U . . .
H3B H 0.6217 0.0107 0.1386 0.029 Uiso 1 1 calc R U . . .
H3C H 0.5024 0.1027 0.1073 0.029 Uiso 1 1 calc R U . . .
N4 N 0.7864(4) 0.1853(3) 0.00874(16) 0.0224(7) Uani 1 1 d . . . . .
H4A H 0.7188 0.1055 -0.0033 0.034 Uiso 1 1 calc R U . . .
H4B H 0.9005 0.1853 -0.0128 0.034 Uiso 1 1 calc R U . . .
H4C H 0.7305 0.2482 -0.0142 0.034 Uiso 1 1 calc DR U . . .
N5 N 0.6473(4) 0.3577(3) 0.12298(18) 0.0200(7) Uani 1 1 d . . . . .
H5A H 0.5516 0.3275 0.0873 0.030 Uiso 1 1 calc R U . . .
H5B H 0.7125 0.4304 0.1033 0.030 Uiso 1 1 calc R U . . .
H5C H 0.6038 0.3782 0.1745 0.030 Uiso 1 1 calc R U . . .
N6 N 0.9597(4) 0.0814(3) 0.13701(18) 0.0188(7) Uani 1 1 d . . . . .
H6A H 0.9751 0.0642 0.1914 0.028 Uiso 1 1 calc R U . . .
H6B H 1.0711 0.1068 0.1146 0.028 Uiso 1 1 calc R U . . .
H6C H 0.9038 0.0079 0.1078 0.028 Uiso 1 1 calc R U . . .
C1 C 0.6710(5) 0.6704(3) 0.3666(2) 0.0166(8) Uani 1 1 d . . . . .
C2 C 0.7577(5) 0.8030(3) 0.3701(2) 0.0168(8) Uani 1 1 d . . . . .
C3 C 0.8237(5) 0.8616(4) 0.4470(2) 0.0198(9) Uani 1 1 d . . . . .
H3 H 0.8834 0.9494 0.4491 0.024 Uiso 1 1 calc R U . . .
C4 C 0.8068(5) 0.7984(4) 0.5206(2) 0.0227(9) Uani 1 1 d . . . . .
H4 H 0.8532 0.8419 0.5721 0.027 Uiso 1 1 calc R U . . .
C5 C 0.7207(5) 0.6702(3) 0.5172(2) 0.0236(9) Uani 1 1 d . . . . .
H5 H 0.7053 0.6249 0.5669 0.028 Uiso 1 1 calc R U . . .
C6 C 0.6578(5) 0.6093(3) 0.4419(2) 0.0214(8) Uani 1 1 d . . . . .
H6 H 0.6021 0.5206 0.4408 0.026 Uiso 1 1 calc R U . . .
C7 C 0.5913(5) 0.5846(4) 0.2916(3) 0.0246(9) Uani 1 1 d . . . . .
C8 C 0.7856(5) 0.8925(4) 0.2990(2) 0.0231(9) Uani 1 1 d . . . . .
C9 C 0.1761(5) 0.7139(3) 0.3417(2) 0.0207(8) Uani 1 1 d . . . . .
C10 C 0.2711(4) 0.8430(3) 0.3543(2) 0.0178(8) Uani 1 1 d . . . . .
C11 C 0.3349(5) 0.8871(4) 0.4349(2) 0.0222(9) Uani 1 1 d . . . . .
H11 H 0.4007 0.9729 0.4433 0.027 Uiso 1 1 calc R U . . .
C12 C 0.3071(5) 0.8121(4) 0.5027(2) 0.0248(9) Uani 1 1 d . . . . .
H12 H 0.3526 0.8456 0.5567 0.030 Uiso 1 1 calc R U . . .
C13 C 0.2113(5) 0.6869(4) 0.4908(2) 0.0279(9) Uani 1 1 d . . . . .
H13 H 0.1883 0.6340 0.5369 0.033 Uiso 1 1 calc R U . . .
C14 C 0.1498(5) 0.6399(4) 0.4117(2) 0.0269(10) Uani 1 1 d . . . . .
H14 H 0.0867 0.5532 0.4043 0.032 Uiso 1 1 calc R U . . .
C15 C 0.0927(5) 0.6436(4) 0.2617(3) 0.0295(10) Uani 1 1 d . . . . .
C16 C 0.3140(5) 0.9443(4) 0.2905(3) 0.0232(9) Uani 1 1 d . . . . .
O1W O 0.8678(4) 0.6057(2) 0.06367(15) 0.0303(7) Uani 1 1 d . . . . .
H1W1 H 0.8139 0.6654 0.0558 0.045 Uiso 1 1 d R U . . .
H2W1 H 0.9210 0.6415 0.1085 0.045 Uiso 1 1 d R U . . .
O2W O 0.2606(4) 0.2678(2) 0.24986(17) 0.0351(7) Uani 1 1 d . . . . .
H1W2 H 0.3375 0.3380 0.2653 0.053 Uiso 1 1 d R U . . .
H2W2 H 0.2934 0.2020 0.2718 0.053 Uiso 1 1 d R U . . .
O3W O 0.3813(5) 0.5773(3) 0.06219(19) 0.0490(9) Uani 1 1 d D . . . .
H1W3 H 0.410(7) 0.582(5) 0.116(2) 0.074 Uiso 1 1 d D U . . .
H2W3 H 0.480(3) 0.636(3) 0.047(3) 0.074 Uiso 1 1 d D U . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N6 91.75(12) . . ?
N1 Co1 N3 179.23(13) . . ?
N6 Co1 N3 88.82(11) . . ?
N1 Co1 N5 89.93(12) . . ?
N6 Co1 N5 177.91(12) . . ?
N3 Co1 N5 89.51(12) . . ?
N1 Co1 N2 88.91(12) . . ?
N6 Co1 N2 89.34(12) . . ?
N3 Co1 N2 90.57(12) . . ?
N5 Co1 N2 91.93(12) . . ?
N1 Co1 N4 90.17(12) . . ?
N6 Co1 N4 89.29(12) . . ?
N3 Co1 N4 90.36(12) . . ?
N5 Co1 N4 89.47(12) . . ?
N2 Co1 N4 178.33(13) . . ?
C6 C1 C2 116.9(3) . . ?
C6 C1 C7 114.3(3) . . ?
C2 C1 C7 128.8(3) . . ?
C3 C2 C1 118.4(3) . . ?
C3 C2 C8 113.9(3) . . ?
C1 C2 C8 127.8(3) . . ?
C4 C3 C2 123.2(3) . . ?
C3 C4 C5 118.3(4) . . ?
C6 C5 C4 119.6(3) . . ?
C5 C6 C1 123.6(3) . . ?
O1 C7 O2 121.2(4) . . ?
O1 C7 C1 118.8(4) . . ?
O2 C7 C1 120.0(3) . . ?
O4 C8 O3 120.6(3) . . ?
O4 C8 C2 119.0(3) . . ?
O3 C8 C2 120.4(3) . . ?
C14 C9 C10 117.5(3) . . ?
C14 C9 C15 113.8(3) . . ?
C10 C9 C15 128.7(3) . . ?
C11 C10 C9 118.3(3) . . ?
C11 C10 C16 113.4(3) . . ?
C9 C10 C16 128.3(3) . . ?
C12 C11 C10 123.0(4) . . ?
C11 C12 C13 118.8(4) . . ?
C14 C13 C12 119.5(4) . . ?
C13 C14 C9 122.9(3) . . ?
O5 C15 O6 121.3(4) . . ?
O5 C15 C9 118.9(4) . . ?
O6 C15 C9 119.8(3) . . ?
O8 C16 O7 120.0(4) . . ?
O8 C16 C10 118.9(3) . . ?
O7 C16 C10 121.1(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 1.956(3) . ?
Co1 N6 1.957(3) . ?
Co1 N3 1.957(3) . ?
Co1 N5 1.960(3) . ?
Co1 N2 1.966(3) . ?
Co1 N4 1.971(3) . ?
O1 C7 1.244(4) . ?
O2 C7 1.276(4) . ?
O3 C8 1.294(4) . ?
O4 C8 1.241(4) . ?
O5 C15 1.222(4) . ?
O6 C15 1.286(5) . ?
O7 C16 1.279(4) . ?
O8 C16 1.245(4) . ?
C1 C6 1.397(5) . ?
C1 C2 1.427(5) . ?
C1 C7 1.508(5) . ?
C2 C3 1.388(5) . ?
C2 C8 1.513(5) . ?
C3 C4 1.383(5) . ?
C4 C5 1.385(5) . ?
C5 C6 1.369(5) . ?
C9 C14 1.399(5) . ?
C9 C10 1.418(5) . ?
C9 C15 1.513(5) . ?
C10 C11 1.394(5) . ?
C10 C16 1.517(5) . ?
C11 C12 1.377(5) . ?
C12 C13 1.386(5) . ?
C13 C14 1.375(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H1O O3 0.89 1.59 2.403(4) 149.2 .
O7 H2O O6 0.88 1.54 2.386(4) 158.5 .
N1 H1A O5 0.91 2.00 2.873(4) 160.1 1_655
N1 H1B O1W 0.91 2.22 3.062(4) 154.3 2_765
N1 H1C Cl1 0.91 2.98 3.568(3) 123.6 1_655
N1 H1C O2W 0.91 2.30 2.988(4) 131.6 1_655
N2 H2A O1 0.91 2.29 3.194(4) 172.2 .
N2 H2B O5 0.91 2.48 2.955(4) 112.5 1_655
N2 H2B O2W 0.91 2.31 3.118(4) 148.2 1_655
N2 H2C O4 0.91 2.14 2.934(4) 145.5 1_545
N3 H3A O8 0.91 2.19 3.044(4) 156.8 1_545
N3 H3B Cl1 0.91 2.79 3.483(3) 133.9 2_655
N3 H3B O3 0.91 2.32 3.039(4) 135.2 1_545
N3 H3C Cl1 0.91 2.39 3.297(3) 173.9 .
N4 H4A Cl1 0.91 2.59 3.384(3) 146.3 2_655
N4 H4B Cl1 0.91 2.99 3.814(3) 152.0 1_655
N4 H4C O3W 0.91 2.26 3.162(4) 172.8 2_665
N5 H5A Cl1 0.91 2.77 3.627(3) 157.7 .
N5 H5B O1W 0.91 2.14 3.051(4) 177.0 .
N5 H5C O1 0.91 2.15 3.039(4) 165.6 .
N6 H6A O4 0.91 2.15 3.001(4) 154.6 1_545
N6 H6B Cl1 0.91 2.48 3.333(3) 155.9 1_655
N6 H6C Cl1 0.91 2.57 3.448(3) 162.1 2_655
O1W H1W1 Cl1 0.79 2.43 3.197(3) 164.2 2_665
O1W H2W1 O6 0.85 1.90 2.724(4) 164.0 1_655
O2W H1W2 O1 0.88 1.98 2.840(3) 164.9 .
O2W H2W2 O8 0.85 2.00 2.843(4) 171.2 1_545
O3W H1W3 O2 0.88(4) 2.03(4) 2.874(4) 158(4) .
O3W H2W3 Cl1 0.924(18) 2.765(18) 3.665(3) 165(2) 2_665
