#------------------------------------------------------------------------------
#$Date: 2020-03-04 04:39:04 +0200 (Wed, 04 Mar 2020) $
#$Revision: 248722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/00/7240018.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_7240018
loop_
_publ_author_name
'Wellm, Carsten'
'Neumann, Tristan'
'Ceglarska, Magdalena'
'Gallo, Gianpiero'
'Rams, Michał'
'Dinnebier, Robert E.'
'Nather, Christian'
_publ_section_title
;
 New isomeric Ni(NCS)2 coordination compounds: crystal structures,
 magnetic properties as well as ex situ and in situ investigations on
 their synthesis and transition behaviour
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00181C
_journal_year                    2020
_chemical_formula_sum            'C17 H20 Cl2 N4 Ni S2'
_chemical_formula_weight         474.10
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-01-28 deposited with the CCDC.	2020-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.894(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8134(6)
_cell_length_b                   14.9609(3)
_cell_length_c                   9.801
_cell_measurement_reflns_used    10318
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.999
_cell_measurement_theta_min      1.907
_cell_volume                     2236.32(10)
_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 0.998
_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  0.0218
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10318
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.907
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_T_max  0.7606
_exptl_absorpt_correction_T_min  0.5825
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape and X-Red 32 (STOE, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2193
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0251
_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)+(0.0388P)²+0.8607P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1967
_reflns_number_total             2193
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00181c2.cif
_cod_data_source_block           cw1829
_cod_original_cell_volume        2236.36(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7240018
_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+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
Ni1 Ni 0.500000 0.08865(2) 0.750000 0.02604(9) Uani 1 2 d S T P . .
S1 S 0.38778(3) 0.03511(3) 0.22107(5) 0.03649(12) Uani 1 1 d . . . . .
C1 C 0.42085(10) 0.06494(10) 0.39790(18) 0.0274(3) Uani 1 1 d . . . . .
N1 N 0.44451(9) 0.08426(9) 0.52264(16) 0.0317(3) Uani 1 1 d . . . . .
N11 N 0.58938(9) 0.18449(9) 0.74745(16) 0.0323(3) Uani 1 1 d . . . . .
C11 C 0.61217(11) 0.25347(12) 0.8426(2) 0.0371(4) Uani 1 1 d . . . . .
H11 H 0.585796 0.258528 0.910975 0.044 Uiso 1 1 calc R U . . .
C12 C 0.67240(13) 0.31835(14) 0.8470(2) 0.0507(5) Uani 1 1 d . . . . .
C13 C 0.70975(15) 0.30815(18) 0.7456(3) 0.0684(7) Uani 1 1 d . . . . .
H13 H 0.751082 0.350754 0.743344 0.082 Uiso 1 1 calc R U . . .
C14 C 0.68720(16) 0.23687(19) 0.6488(3) 0.0662(7) Uani 1 1 d . . . . .
H14 H 0.713257 0.229492 0.580339 0.079 Uiso 1 1 calc R U . . .
C15 C 0.62718(13) 0.17671(14) 0.6517(2) 0.0455(4) Uani 1 1 d . . . . .
H15 H 0.611556 0.127713 0.583727 0.055 Uiso 1 1 calc R U . . .
C16 C 0.69415(18) 0.39473(15) 0.9563(3) 0.0691(7) Uani 1 1 d D . . . .
H16A H 0.757958 0.394804 1.020903 0.083 Uiso 0.55 1 calc R U P A 1
H16B H 0.663245 0.386400 1.021840 0.083 Uiso 0.55 1 calc R U P A 1
H16C H 0.701432 0.371114 1.055179 0.083 Uiso 0.45 1 calc R U P B 2
H16D H 0.751051 0.420587 0.968936 0.083 Uiso 0.45 1 calc R U P B 2
C17' C 0.6678(6) 0.4848(5) 0.8753(12) 0.100(3) Uani 0.55 1 d D . P C 1
H17A H 0.701511 0.495284 0.816139 0.149 Uiso 0.55 1 calc R U P C 1
H17B H 0.679859 0.532664 0.949733 0.149 Uiso 0.55 1 calc R U P C 1
H17C H 0.605034 0.484161 0.808396 0.149 Uiso 0.55 1 calc R U P C 1
C17 C 0.6273(8) 0.4675(6) 0.9109(15) 0.120(5) Uani 0.45 1 d D . P C 2
H17D H 0.618613 0.490703 0.812134 0.180 Uiso 0.45 1 calc R U P C 2
H17E H 0.647699 0.515817 0.985263 0.180 Uiso 0.45 1 calc R U P C 2
H17F H 0.571773 0.443789 0.905667 0.180 Uiso 0.45 1 calc R U P C 2
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'
Ni Ni 0.3393 1.1124 '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'
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 Ni1 N1 176.28(8) . 2_656 ?
N1 Ni1 N11 90.55(6) . . ?
N1 Ni1 N11 92.01(6) 2_656 . ?
N1 Ni1 N11 92.01(5) . 2_656 ?
N1 Ni1 N11 90.55(6) 2_656 2_656 ?
N11 Ni1 N11 93.10(8) . 2_656 ?
N1 Ni1 S1 83.02(4) . 6_556 ?
N1 Ni1 S1 94.29(4) 2_656 6_556 ?
N11 Ni1 S1 173.02(4) . 6_556 ?
N11 Ni1 S1 89.85(4) 2_656 6_556 ?
N1 Ni1 S1 94.29(4) . 5_656 ?
N1 Ni1 S1 83.02(4) 2_656 5_656 ?
N11 Ni1 S1 89.85(4) . 5_656 ?
N11 Ni1 S1 173.02(4) 2_656 5_656 ?
S1 Ni1 S1 87.94(2) 6_556 5_656 ?
C1 S1 Ni1 99.92(5) . 5_656 ?
N1 C1 S1 178.75(15) . . ?
C1 N1 Ni1 166.06(13) . . ?
C11 N11 C15 118.32(16) . . ?
C11 N11 Ni1 121.34(12) . . ?
C15 N11 Ni1 120.32(13) . . ?
N11 C11 C12 123.60(18) . . ?
C13 C12 C11 116.3(2) . . ?
C13 C12 C16 123.1(2) . . ?
C11 C12 C16 120.6(2) . . ?
C14 C13 C12 120.2(2) . . ?
C15 C14 C13 119.5(2) . . ?
N11 C15 C14 122.0(2) . . ?
C17 C16 C12 114.6(5) . . ?
C12 C16 C17' 111.7(5) . . ?
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
Ni1 N1 2.0224(14) . ?
Ni1 N1 2.0224(14) 2_656 ?
Ni1 N11 2.0847(14) . ?
Ni1 N11 2.0848(14) 2_656 ?
Ni1 S1 2.5726(5) 6_556 ?
Ni1 S1 2.5726(5) 5_656 ?
S1 C1 1.6434(17) . ?
C1 N1 1.152(2) . ?
N11 C11 1.334(2) . ?
N11 C15 1.342(2) . ?
C11 C12 1.390(3) . ?
C12 C13 1.390(4) . ?
C12 C16 1.502(3) . ?
C13 C14 1.370(4) . ?
C14 C15 1.361(3) . ?
C16 C17 1.491(10) . ?
C16 C17' 1.532(7) . ?
