#------------------------------------------------------------------------------
#$Date: 2020-03-04 04:39:04 +0200 (Wed, 04 Mar 2020) $
#$Revision: 248722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/00/7240017.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_7240017
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            'C16 H22 N4 Ni O2 S2'
_chemical_formula_weight         425.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 100.883(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1142(5)
_cell_length_b                   14.0364(6)
_cell_length_c                   7.8828(4)
_cell_measurement_reflns_used    7715
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.005
_cell_measurement_theta_min      2.275
_cell_volume                     990.31(9)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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  0.1104
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7715
_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         26.005
_diffrn_reflns_theta_min         2.275
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  0.9148
_exptl_absorpt_correction_T_min  0.7989
_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    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.1252
_exptl_crystal_size_mid          0.0916
_exptl_crystal_size_min          0.0617
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.026(7)
_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   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0583
_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)+(0.1189P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1719
_reflns_number_total             1945
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00181c2.cif
_cod_data_source_block           cw1246a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Numerical' was
changed to 'numerical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7240017
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.500000 0.500000 0.0399(3) Uani 1 2 d S . P . .
N1 N 0.5822(3) 0.42908(17) 0.7247(3) 0.0480(6) Uani 1 1 d . . . . .
C1 C 0.6305(3) 0.38307(18) 0.8423(3) 0.0395(6) Uani 1 1 d . . . . .
S1 S 0.70218(9) 0.31697(5) 1.01059(9) 0.0480(3) Uani 1 1 d . . . . .
N11 N 0.3107(3) 0.41151(17) 0.4616(3) 0.0445(6) Uani 1 1 d . . . . .
C11 C 0.3237(3) 0.31695(19) 0.4871(4) 0.0462(7) Uani 1 1 d . . . . .
H11 H 0.420768 0.291893 0.527987 0.055 Uiso 1 1 calc R U . . .
C12 C 0.2067(3) 0.2545(2) 0.4583(4) 0.0491(7) Uani 1 1 d . . . . .
C13 C 0.0647(3) 0.2921(2) 0.4011(5) 0.0571(8) Uani 1 1 d . . . . .
H13 H -0.020269 0.251565 0.380486 0.069 Uiso 1 1 calc R U . . .
C14 C 0.0489(3) 0.3892(2) 0.3746(5) 0.0578(8) Uani 1 1 d . . . . .
H14 H -0.046994 0.416264 0.335145 0.069 Uiso 1 1 calc R U . . .
C15 C 0.1732(3) 0.4459(2) 0.4060(4) 0.0487(7) Uani 1 1 d . . . . .
H15 H 0.161336 0.512537 0.387471 0.058 Uiso 1 1 calc R U . . .
C16 C 0.2376(4) 0.1490(2) 0.4887(5) 0.0660(10) Uani 1 1 d . . . . .
H16A H 0.336397 0.134623 0.459835 0.079 Uiso 1 1 calc R U . . .
H16B H 0.244859 0.135984 0.613460 0.079 Uiso 1 1 calc R U . . .
C17 C 0.1286(7) 0.0834(3) 0.3924(7) 0.0992(18) Uani 1 1 d . . . . .
H17A H 0.034112 0.088780 0.433898 0.149 Uiso 1 1 calc R U . . .
H17B H 0.166225 0.018034 0.409397 0.149 Uiso 1 1 calc R U . . .
H17C H 0.112149 0.099366 0.269249 0.149 Uiso 1 1 calc R U . . .
O1 O 0.6183(3) 0.40322(14) 0.3707(3) 0.0515(5) Uani 1 1 d . . . . .
H1A H 0.612980 0.402444 0.263161 0.077 Uiso 1 1 d R U . . .
H2A H 0.627133 0.347324 0.409331 0.077 Uiso 1 1 d R 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'
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'
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 Ni1 N1 180.0 3_666 . ?
N1 Ni1 N11 90.36(10) 3_666 . ?
N1 Ni1 N11 89.64(10) . . ?
N1 Ni1 N11 89.64(10) 3_666 3_666 ?
N1 Ni1 N11 90.36(10) . 3_666 ?
N11 Ni1 N11 180.0 . 3_666 ?
N1 Ni1 O1 91.83(9) 3_666 . ?
N1 Ni1 O1 88.17(9) . . ?
N11 Ni1 O1 91.73(9) . . ?
N11 Ni1 O1 88.27(9) 3_666 . ?
N1 Ni1 O1 88.17(9) 3_666 3_666 ?
N1 Ni1 O1 91.83(9) . 3_666 ?
N11 Ni1 O1 88.27(9) . 3_666 ?
N11 Ni1 O1 91.73(9) 3_666 3_666 ?
O1 Ni1 O1 180.0 . 3_666 ?
C1 N1 Ni1 174.3(2) . . ?
N1 C1 S1 179.3(3) . . ?
C15 N11 C11 117.1(2) . . ?
C15 N11 Ni1 121.82(19) . . ?
C11 N11 Ni1 121.02(18) . . ?
N11 C11 C12 124.4(2) . . ?
C11 C12 C13 117.3(3) . . ?
C11 C12 C16 118.9(3) . . ?
C13 C12 C16 123.7(3) . . ?
C14 C13 C12 119.2(3) . . ?
C15 C14 C13 119.1(3) . . ?
N11 C15 C14 122.8(3) . . ?
C17 C16 C12 116.4(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
Ni1 N1 2.047(3) 3_666 ?
Ni1 N1 2.047(3) . ?
Ni1 N11 2.101(2) . ?
Ni1 N11 2.101(2) 3_666 ?
Ni1 O1 2.112(2) . ?
Ni1 O1 2.112(2) 3_666 ?
N1 C1 1.147(4) . ?
C1 S1 1.649(3) . ?
N11 C15 1.337(4) . ?
N11 C11 1.344(4) . ?
C11 C12 1.367(4) . ?
C12 C13 1.391(4) . ?
C12 C16 1.518(4) . ?
C13 C14 1.383(4) . ?
C14 C15 1.368(4) . ?
C16 C17 1.458(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
_geom_hbond_publ_flag
C11 H11 S1 0.95 3.01 3.902(3) 156.8 4_565 yes
O1 H1A S1 0.84 2.58 3.306(2) 144.8 1_554 yes
O1 H2A S1 0.84 2.49 3.322(2) 169.0 4_565 yes
