#------------------------------------------------------------------------------
#$Date: 2021-01-05 09:37:40 +0200 (Tue, 05 Jan 2021) $
#$Revision: 260522 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/62/7706294.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_7706294
loop_
_publ_author_name
'Jochim, Aleksej'
'Rams, Michał'
'Böhme, Michael'
'Ceglarska, Magdalena'
'Plass, Winfried'
'Näther, Christian'
_publ_section_title
;
 Thermodynamically metastable chain and stable layered Co(NCS)₂
 coordination polymers: thermodynamic relations and magnetic properties.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15310
_journal_page_last               15322
_journal_paper_doi               10.1039/d0dt03227a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C14 H16 Br2 Co N4 O2 S2'
_chemical_formula_weight         555.18
_chemical_properties_physical    Air-sensitive,Heat-sensitive
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-11 deposited with the CCDC.	2020-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                73.836(5)
_cell_angle_beta                 80.371(5)
_cell_angle_gamma                79.875(5)
_cell_formula_units_Z            1
_cell_length_a                   6.8581(4)
_cell_length_b                   7.6865(5)
_cell_length_c                   10.2102(6)
_cell_measurement_reflns_used    8394
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.389
_cell_measurement_theta_min      2.093
_cell_volume                     504.90(6)
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_collection       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8394
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.389
_diffrn_reflns_theta_min         2.093
_exptl_absorpt_coefficient_mu    5.028
_exptl_absorpt_correction_T_max  0.4362
_exptl_absorpt_correction_T_min  0.2767
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red 32 (STOE, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       block
_exptl_crystal_F_000             273
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0335
_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)+(0.0459P)²+0.1286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2123
_reflns_number_total             2536
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03227a2.cif
_cod_data_source_block           ss2188f
_cod_database_code               7706294
_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.
;
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 0.000000 0.500000 0.500000 0.02872(12) Uani 1 2 d S . P . .
N1 N 0.1257(3) 0.5828(3) 0.6399(2) 0.0350(5) Uani 1 1 d . . . . .
C1 C 0.2367(4) 0.6143(3) 0.7016(3) 0.0315(5) Uani 1 1 d . . . . .
S1 S 0.39286(11) 0.65922(11) 0.78940(8) 0.04084(17) Uani 1 1 d . . . . .
O1 O 0.2668(3) 0.3189(3) 0.4705(2) 0.0377(4) Uani 1 1 d . . . . .
H1 H 0.343869 0.343243 0.396682 0.056 Uiso 1 1 d R U . . .
C2 C 0.3875(5) 0.2223(4) 0.5772(3) 0.0478(7) Uani 1 1 d . . . . .
H2A H 0.474367 0.303565 0.589549 0.072 Uiso 1 1 calc R U . . .
H2B H 0.469549 0.115938 0.551739 0.072 Uiso 1 1 calc R U . . .
H2C H 0.301061 0.181394 0.663341 0.072 Uiso 1 1 calc R U . . .
N11 N 0.1029(3) 0.7210(3) 0.3342(2) 0.0314(4) Uani 1 1 d . . . . .
C11 C 0.1111(4) 0.8784(3) 0.3640(3) 0.0348(5) Uani 1 1 d . . . . .
H11 H 0.082037 0.882377 0.457545 0.052 Uiso 1 1 calc R U . . .
C12 C 0.1589(4) 1.0346(4) 0.2675(3) 0.0370(6) Uani 1 1 d . . . . .
H12 H 0.161795 1.143727 0.293238 0.044 Uiso 1 1 calc R U . . .
C13 C 0.2026(4) 1.0273(4) 0.1318(3) 0.0352(5) Uani 1 1 d . . . . .
C14 C 0.1971(4) 0.8680(4) 0.0974(3) 0.0373(6) Uani 1 1 d . . . . .
H14 H 0.227126 0.860750 0.004671 0.045 Uiso 1 1 calc R U . . .
C15 C 0.1467(4) 0.7183(4) 0.2017(3) 0.0345(5) Uani 1 1 d . . . . .
H15 H 0.142745 0.607764 0.178297 0.041 Uiso 1 1 calc R U . . .
Br1 Br 0.26929(5) 1.24037(4) -0.00233(3) 0.04635(12) Uani 1 1 d . . . . .
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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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 N1 180.0 . 2_566 ?
N1 Co1 O1 89.46(8) . . ?
N1 Co1 O1 90.54(8) 2_566 . ?
N1 Co1 O1 90.54(8) . 2_566 ?
N1 Co1 O1 89.46(8) 2_566 2_566 ?
O1 Co1 O1 180.00(7) . 2_566 ?
N1 Co1 N11 91.17(8) . . ?
N1 Co1 N11 88.83(8) 2_566 . ?
O1 Co1 N11 92.87(8) . . ?
O1 Co1 N11 87.13(8) 2_566 . ?
N1 Co1 N11 88.83(8) . 2_566 ?
N1 Co1 N11 91.17(8) 2_566 2_566 ?
O1 Co1 N11 87.13(8) . 2_566 ?
O1 Co1 N11 92.87(8) 2_566 2_566 ?
N11 Co1 N11 180.0 . 2_566 ?
C1 N1 Co1 164.1(2) . . ?
N1 C1 S1 179.7(3) . . ?
C2 O1 Co1 124.06(18) . . ?
C2 O1 H1 107.4 . . ?
Co1 O1 H1 119.6 . . ?
O1 C2 H2A 109.5 . . ?
O1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C11 N11 C15 116.9(2) . . ?
C11 N11 Co1 117.58(17) . . ?
C15 N11 Co1 125.38(17) . . ?
N11 C11 C12 124.0(3) . . ?
N11 C11 H11 118.0 . . ?
C12 C11 H11 118.0 . . ?
C11 C12 C13 117.7(2) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
C14 C13 C12 120.0(2) . . ?
C14 C13 Br1 121.7(2) . . ?
C12 C13 Br1 118.3(2) . . ?
C13 C14 C15 118.1(3) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
N11 C15 C14 123.4(2) . . ?
N11 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
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 2.074(2) . ?
Co1 N1 2.074(2) 2_566 ?
Co1 O1 2.1286(18) . ?
Co1 O1 2.1286(18) 2_566 ?
Co1 N11 2.161(2) . ?
Co1 N11 2.161(2) 2_566 ?
N1 C1 1.160(3) . ?
C1 S1 1.641(3) . ?
O1 C2 1.435(4) . ?
O1 H1 0.8400 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N11 C11 1.339(3) . ?
N11 C15 1.341(3) . ?
C11 C12 1.376(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.373(4) . ?
C13 Br1 1.890(3) . ?
C14 C15 1.383(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
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
_geom_hbond_publ_flag
O1 H1 S1 0.84 2.39 3.215(2) 165.9 2_666 yes
C11 H11 N1 0.95 2.53 3.091(4) 117.7 . yes
C14 H14 S1 0.95 2.99 3.861(3) 152.4 1_554 yes
