#------------------------------------------------------------------------------
#$Date: 2021-01-05 09:37:40 +0200 (Tue, 05 Jan 2021) $
#$Revision: 260522 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/62/7706295.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_7706295
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            'C12 H8 Br2 Co N4 S2'
_chemical_formula_weight         491.09
_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   geom
_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                73.304(3)
_cell_angle_beta                 83.016(3)
_cell_angle_gamma                80.318(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0951(3)
_cell_length_b                   9.4346(4)
_cell_length_c                   10.8479(4)
_cell_measurement_reflns_used    12527
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.005
_cell_measurement_theta_min      1.966
_cell_volume                     779.91(5)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12527
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.005
_diffrn_reflns_theta_min         1.966
_exptl_absorpt_coefficient_mu    6.487
_exptl_absorpt_correction_T_max  0.4617
_exptl_absorpt_correction_T_min  0.1879
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-butanol/n-heptane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.0078(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         3758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0325
_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)+(0.0484P)²+0.4474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3216
_reflns_number_total             3758
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03227a2.cif
_cod_data_source_block           aj2485d
_cod_database_code               7706295
_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 0.500000 0.500000 0.500000 0.02849(13) Uani 1 2 d S . P . .
Co2 Co 0.000000 1.000000 0.500000 0.02687(13) Uani 1 2 d S . P . .
N1 N 0.0368(3) 0.7687(2) 0.5415(2) 0.0300(5) Uani 1 1 d . . . . .
C1 C 0.1031(3) 0.6465(3) 0.5746(3) 0.0277(5) Uani 1 1 d . . . . .
S1 S 0.20072(9) 0.47437(7) 0.62035(7) 0.03117(16) Uani 1 1 d . . . . .
N2 N 0.4376(3) 0.7257(3) 0.4233(2) 0.0329(5) Uani 1 1 d . . . . .
C2 C 0.3788(3) 0.8495(3) 0.4089(3) 0.0293(5) Uani 1 1 d . . . . .
S2 S 0.29734(9) 1.02544(7) 0.38578(7) 0.03360(16) Uani 1 1 d . . . . .
N11 N 0.4124(3) 0.4562(3) 0.3362(2) 0.0325(5) Uani 1 1 d . . . . .
C11 C 0.2654(4) 0.5258(4) 0.2901(3) 0.0389(7) Uani 1 1 d . . . . .
H11 H 0.198161 0.591678 0.333986 0.047 Uiso 1 1 calc R U . . .
C12 C 0.2060(4) 0.5076(4) 0.1828(3) 0.0401(7) Uani 1 1 d . . . . .
H12 H 0.099770 0.557874 0.154316 0.048 Uiso 1 1 calc R U . . .
C13 C 0.3048(4) 0.4148(3) 0.1184(3) 0.0360(6) Uani 1 1 d . . . . .
C14 C 0.4548(4) 0.3371(4) 0.1643(3) 0.0400(7) Uani 1 1 d . . . . .
H14 H 0.522839 0.269793 0.122289 0.048 Uiso 1 1 calc R U . . .
C15 C 0.5022(4) 0.3613(3) 0.2740(3) 0.0371(6) Uani 1 1 d . . . . .
H15 H 0.604603 0.307311 0.307276 0.045 Uiso 1 1 calc R U . . .
Br11 Br 0.23975(5) 0.39674(4) -0.03817(3) 0.04770(12) Uani 1 1 d . . . . .
N21 N 0.0973(3) 0.9788(3) 0.6820(2) 0.0307(5) Uani 1 1 d . . . . .
C21 C 0.1948(4) 1.0743(3) 0.6953(3) 0.0361(6) Uani 1 1 d . . . . .
H21 H 0.222468 1.151948 0.621471 0.043 Uiso 1 1 calc R U . . .
C22 C 0.2571(4) 1.0659(4) 0.8107(3) 0.0381(6) Uani 1 1 d . . . . .
H22 H 0.325700 1.135677 0.816757 0.046 Uiso 1 1 calc R U . . .
C23 C 0.2158(4) 0.9518(4) 0.9173(3) 0.0366(6) Uani 1 1 d . . . . .
C24 C 0.1176(4) 0.8517(4) 0.9055(3) 0.0414(7) Uani 1 1 d . . . . .
H24 H 0.089769 0.772012 0.977485 0.050 Uiso 1 1 calc R U . . .
C25 C 0.0604(4) 0.8700(3) 0.7862(3) 0.0369(6) Uani 1 1 d . . . . .
H25 H -0.008669 0.801584 0.778084 0.044 Uiso 1 1 calc R U . . .
Br21 Br 0.29229(5) 0.93240(5) 1.07987(3) 0.05100(13) 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'
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
N2 Co1 N2 180.0 2_666 . ?
N2 Co1 N11 89.10(10) 2_666 . ?
N2 Co1 N11 90.90(10) . . ?
N2 Co1 N11 90.90(10) 2_666 2_666 ?
N2 Co1 N11 89.10(10) . 2_666 ?
N11 Co1 N11 180.00(13) . 2_666 ?
N2 Co1 S1 92.17(7) 2_666 2_666 ?
N2 Co1 S1 87.83(7) . 2_666 ?
N11 Co1 S1 90.77(7) . 2_666 ?
N11 Co1 S1 89.23(7) 2_666 2_666 ?
N2 Co1 S1 87.83(7) 2_666 . ?
N2 Co1 S1 92.17(7) . . ?
N11 Co1 S1 89.23(7) . . ?
N11 Co1 S1 90.77(7) 2_666 . ?
S1 Co1 S1 180.0 2_666 . ?
N1 Co2 N1 180.0 2_576 . ?
N1 Co2 N21 88.55(9) 2_576 2_576 ?
N1 Co2 N21 91.45(9) . 2_576 ?
N1 Co2 N21 91.45(9) 2_576 . ?
N1 Co2 N21 88.55(9) . . ?
N21 Co2 N21 180.0 2_576 . ?
N1 Co2 S2 86.35(7) 2_576 . ?
N1 Co2 S2 93.64(7) . . ?
N21 Co2 S2 90.19(7) 2_576 . ?
N21 Co2 S2 89.81(7) . . ?
N1 Co2 S2 93.65(7) 2_576 2_576 ?
N1 Co2 S2 86.36(7) . 2_576 ?
N21 Co2 S2 89.80(7) 2_576 2_576 ?
N21 Co2 S2 90.20(7) . 2_576 ?
S2 Co2 S2 180.0 . 2_576 ?
C1 N1 Co2 159.2(2) . . ?
N1 C1 S1 178.8(3) . . ?
C1 S1 Co1 102.17(10) . . ?
C2 N2 Co1 163.0(2) . . ?
N2 C2 S2 178.9(3) . . ?
C2 S2 Co2 101.09(10) . . ?
C11 N11 C15 116.5(3) . . ?
C11 N11 Co1 121.1(2) . . ?
C15 N11 Co1 122.4(2) . . ?
N11 C11 C12 123.9(3) . . ?
C13 C12 C11 117.9(3) . . ?
C12 C13 C14 120.4(3) . . ?
C12 C13 Br11 120.3(2) . . ?
C14 C13 Br11 119.3(2) . . ?
C13 C14 C15 117.2(3) . . ?
N11 C15 C14 124.0(3) . . ?
C25 N21 C21 117.6(3) . . ?
C25 N21 Co2 120.6(2) . . ?
C21 N21 Co2 121.79(19) . . ?
N21 C21 C22 123.5(3) . . ?
C21 C22 C23 117.5(3) . . ?
C24 C23 C22 120.0(3) . . ?
C24 C23 Br21 119.3(2) . . ?
C22 C23 Br21 120.7(2) . . ?
C23 C24 C25 118.2(3) . . ?
N21 C25 C24 123.2(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 N2 2.051(2) 2_666 ?
Co1 N2 2.051(2) . ?
Co1 N11 2.158(2) . ?
Co1 N11 2.158(2) 2_666 ?
Co1 S1 2.6228(7) 2_666 ?
Co1 S1 2.6228(7) . ?
Co2 N1 2.074(2) 2_576 ?
Co2 N1 2.074(2) . ?
Co2 N21 2.158(2) 2_576 ?
Co2 N21 2.158(2) . ?
Co2 S2 2.5855(7) . ?
Co2 S2 2.5855(7) 2_576 ?
N1 C1 1.160(4) . ?
C1 S1 1.646(3) . ?
N2 C2 1.158(4) . ?
C2 S2 1.639(3) . ?
N11 C11 1.338(4) . ?
N11 C15 1.340(4) . ?
C11 C12 1.377(5) . ?
C12 C13 1.369(5) . ?
C13 C14 1.377(5) . ?
C13 Br11 1.899(3) . ?
C14 C15 1.383(4) . ?
N21 C25 1.332(4) . ?
N21 C21 1.341(4) . ?
C21 C22 1.383(4) . ?
C22 C23 1.385(4) . ?
C23 C24 1.373(5) . ?
C23 Br21 1.889(3) . ?
C24 C25 1.382(4) . ?
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
C11 H11 S1 0.95 2.98 3.460(3) 112.4 . yes
C12 H12 Br11 0.95 3.08 3.970(3) 157.5 2_565 yes
C21 H21 S1 0.95 3.01 3.633(3) 124.1 1_565 yes
C25 H25 N1 0.95 2.65 3.104(4) 110.1 . yes
