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#$Date: 2022-06-06 04:45:10 +0300 (Mon, 06 Jun 2022) $
#$Revision: 275781 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/49/1564952.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_1564952
loop_
_publ_author_name
'Rotärmel, Thomas'
'Becker, Jonathan'
'Schindler, Siegfried'
_publ_section_title
;
 Syntheses and investigation of metal complexes with macrocyclic
 polythioether ligands.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              70
_journal_page_last               85
_journal_paper_doi               10.1039/d1fd00062d
_journal_volume                  234
_journal_year                    2022
_chemical_formula_sum            'C12 H23 Cl2 Co N S4'
_chemical_formula_weight         439.38
_chemical_name_common            {[CoII(14-S₄)(MeCN)(Cl2)]}n
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2021-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.733(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.553(4)
_cell_length_b                   8.7583(18)
_cell_length_c                   9.884(2)
_cell_measurement_reflns_used    6181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.92
_cell_measurement_theta_min      2.51
_cell_volume                     1844.1(6)
_computing_cell_refinement       'SAINT 8.40A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2019.1-0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.40A (Bruker-AXS, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker PHOTON100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0914
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23543
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         2.514
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    1.663
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2(Sheldrick, 2016)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0327
_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)+(0.0265P)²+2.8771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2095
_reflns_number_total             2697
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1fd00062d2.cif
_cod_data_source_block           D20551
_cod_depositor_comments
'Adding full bibliography for 1564950--1564960.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1564952
_shelx_shelxl_version_number     2018/3
_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   0.752
_shelx_estimated_absorpt_t_max   0.828
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.500000 0.31947(5) 0.250000 0.01019(10) Uani 1 2 d S T P . .
Cl1 Cl 0.55893(2) 0.19669(6) 0.11255(5) 0.01486(11) Uani 1 1 d . . . . .
S1 S 0.58527(2) 0.32134(6) 0.46208(5) 0.01150(11) Uani 1 1 d . . . . .
S2 S 0.73331(2) 0.60735(6) 0.31834(5) 0.01357(12) Uani 1 1 d . . . . .
C1 C 0.64682(10) 0.4607(2) 0.4524(2) 0.0128(4) Uani 1 1 d . . . . .
H1A H 0.629910 0.563541 0.466622 0.015 Uiso 1 1 calc R U . . .
H1B H 0.681429 0.441174 0.528475 0.015 Uiso 1 1 calc R U . . .
C2 C 0.67376(9) 0.4614(2) 0.3190(2) 0.0126(4) Uani 1 1 d . . . . .
H2A H 0.639498 0.479509 0.241928 0.015 Uiso 1 1 calc R U . . .
H2B H 0.692308 0.360193 0.305356 0.015 Uiso 1 1 calc R U . . .
C3 C 0.79349(9) 0.5475(2) 0.4561(2) 0.0128(4) Uani 1 1 d . . . . .
H3A H 0.826908 0.626052 0.468790 0.015 Uiso 1 1 calc R U . . .
H3B H 0.774947 0.542610 0.541650 0.015 Uiso 1 1 calc R U . . .
C4 C 0.82318(10) 0.3940(2) 0.4338(2) 0.0133(4) Uani 1 1 d . . . . .
H4A H 0.840496 0.395590 0.346574 0.016 Uiso 1 1 calc R U . . .
H4B H 0.790909 0.312857 0.427753 0.016 Uiso 1 1 calc R U . . .
C5 C 0.87550(10) 0.3599(2) 0.5519(2) 0.0124(4) Uani 1 1 d . . . . .
H5A H 0.857620 0.360812 0.638423 0.015 Uiso 1 1 calc R U . . .
H5B H 0.907080 0.442627 0.557264 0.015 Uiso 1 1 calc R U . . .
N11 N 0.500000 0.5495(3) 0.250000 0.0142(5) Uani 1 2 d S T P . .
C11 C 0.500000 0.6788(4) 0.250000 0.0167(6) Uani 1 2 d S T P . .
C12 C 0.500000 0.8439(4) 0.250000 0.0397(11) Uani 1 2 d S T P . .
H12A H 0.508352 0.881220 0.161033 0.060 Uiso 0.5 1 calc R U P . .
H12B H 0.532681 0.881220 0.322278 0.060 Uiso 0.5 1 calc R U P . .
H12C H 0.458967 0.881220 0.266690 0.060 Uiso 0.5 1 calc R U P . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
N11 Co1 Cl1 118.319(17) . . ?
N11 Co1 Cl1 118.319(17) . 2_655 ?
Cl1 Co1 Cl1 123.36(3) . 2_655 ?
N11 Co1 S1 89.635(15) . . ?
Cl1 Co1 S1 95.48(2) . . ?
Cl1 Co1 S1 84.87(2) 2_655 . ?
N11 Co1 S1 89.636(15) . 2_655 ?
Cl1 Co1 S1 84.87(2) . 2_655 ?
Cl1 Co1 S1 95.48(2) 2_655 2_655 ?
S1 Co1 S1 179.27(3) . 2_655 ?
C5 S1 C1 103.38(10) 7_656 . ?
C5 S1 Co1 102.49(7) 7_656 . ?
C1 S1 Co1 113.53(7) . . ?
C3 S2 C2 102.72(10) . . ?
C2 C1 S1 115.28(15) . . ?
C2 C1 H1A 108.5 . . ?
S1 C1 H1A 108.5 . . ?
C2 C1 H1B 108.5 . . ?
S1 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
C1 C2 S2 111.74(14) . . ?
C1 C2 H2A 109.3 . . ?
S2 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
S2 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 S2 114.64(14) . . ?
C4 C3 H3A 108.6 . . ?
S2 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
S2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 C5 109.96(17) . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 C5 S1 114.36(14) . 7_656 ?
C4 C5 H5A 108.7 . . ?
S1 C5 H5A 108.7 7_656 . ?
C4 C5 H5B 108.7 . . ?
S1 C5 H5B 108.7 7_656 . ?
H5A C5 H5B 107.6 . . ?
C11 N11 Co1 180.0 . . ?
N11 C11 C12 180.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12A 109.469(7) . 2_655 ?
H12A C12 H12A 141.1 . 2_655 ?
H12B C12 H12A 56.2 . 2_655 ?
H12C C12 H12A 56.3 . 2_655 ?
C11 C12 H12B 109.469(10) . 2_655 ?
H12A C12 H12B 56.3 . 2_655 ?
H12B C12 H12B 141.1 . 2_655 ?
H12C C12 H12B 56.2 . 2_655 ?
H12A C12 H12B 109.5 2_655 2_655 ?
C11 C12 H12C 109.47(2) . 2_655 ?
H12A C12 H12C 56.3 . 2_655 ?
H12B C12 H12C 56.2 . 2_655 ?
H12C C12 H12C 141.1 . 2_655 ?
H12A C12 H12C 109.5 2_655 2_655 ?
H12B C12 H12C 109.5 2_655 2_655 ?
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 N11 2.015(3) . ?
Co1 Cl1 2.2669(6) . ?
Co1 Cl1 2.2669(6) 2_655 ?
Co1 S1 2.5695(7) . ?
Co1 S1 2.5695(7) 2_655 ?
S1 C5 1.813(2) 7_656 ?
S1 C1 1.816(2) . ?
S2 C3 1.809(2) . ?
S2 C2 1.812(2) . ?
C1 C2 1.519(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.519(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.525(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N11 C11 1.132(4) . ?
C11 C12 1.446(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12A 0.9800 2_655 ?
C12 H12B 0.9800 2_655 ?
C12 H12C 0.9800 2_655 ?
