#------------------------------------------------------------------------------
#$Date: 2022-04-28 01:44:10 +0300 (Thu, 28 Apr 2022) $
#$Revision: 274725 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/48/7244861.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_7244861
loop_
_publ_author_name
'Qian, yin'
'Wang, Yi-Ming'
'Xu, Lei'
'Yao, Wanwan'
'Shao, Dong-Sheng'
'Ren, XiaoMing'
_publ_section_title
;
 Formation of Organic Ion Cocrystals, Phase Transition and Ion Conduction
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00156J
_journal_year                    2022
_chemical_formula_sum            'C16 H24 N6 Ni S4'
_chemical_formula_weight         487.36
_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-2016/6
_audit_update_record
;
2021-04-12 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                114.353(3)
_cell_angle_beta                 103.978(3)
_cell_angle_gamma                100.933(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0311(6)
_cell_length_b                   9.2690(7)
_cell_length_c                   9.4907(7)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      40.77
_cell_measurement_theta_min      4.43
_cell_volume                     590.19(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10745
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         4.428
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             254
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0505
_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)+(0.0291P)²+1.0636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1766
_reflns_number_total             2070
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00156j2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7244861
_shelx_shelxl_version_number     2016/6
_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
Ni1 Ni 0.000000 0.000000 0.000000 0.0398(3) Uani 1 2 d S . P . .
S1 S 0.17993(13) 0.11343(12) 0.25658(11) 0.0504(3) Uani 1 1 d . . . . .
S2 S -0.04084(14) 0.23545(13) 0.03503(11) 0.0550(3) Uani 1 1 d . . . . .
N1 N 0.3704(6) 0.5157(6) 0.6468(5) 0.0831(13) Uani 1 1 d . . . . .
N2 N 0.0985(7) 0.6796(6) 0.3552(6) 0.0821(12) Uani 1 1 d . . . . .
N3 N 0.6136(4) 0.8558(4) 0.2140(4) 0.0486(7) Uani 1 1 d . . . . .
C1 C 0.2870(6) 0.4310(5) 0.5095(5) 0.0571(10) Uani 1 1 d . . . . .
C2 C 0.1829(5) 0.3206(5) 0.3389(4) 0.0459(8) Uani 1 1 d . . . . .
C3 C 0.0860(5) 0.3717(5) 0.2410(5) 0.0485(9) Uani 1 1 d . . . . .
C4 C 0.0921(6) 0.5424(6) 0.3064(5) 0.0587(10) Uani 1 1 d . . . . .
C5 C 0.4761(7) 0.8010(10) 0.2762(8) 0.096(2) Uani 1 1 d . . . . .
H5A H 0.458627 0.686233 0.249929 0.143 Uiso 1 1 calc R U . . .
H5B H 0.363397 0.811187 0.224930 0.143 Uiso 1 1 calc R U . . .
H5C H 0.516602 0.869926 0.394046 0.143 Uiso 1 1 calc R U . . .
C6 C 0.5480(10) 0.7574(9) 0.0331(7) 0.105(2) Uani 1 1 d . . . . .
H6A H 0.635530 0.796785 -0.007192 0.158 Uiso 1 1 calc R U . . .
H6B H 0.434627 0.769461 -0.013408 0.158 Uiso 1 1 calc R U . . .
H6C H 0.530837 0.641447 0.001410 0.158 Uiso 1 1 calc R U . . .
C7 C 0.6357(12) 1.0330(9) 0.2449(12) 0.127(3) Uani 1 1 d . . . . .
H7A H 0.674769 1.107013 0.361781 0.191 Uiso 1 1 calc R U . . .
H7B H 0.521597 1.038217 0.189823 0.191 Uiso 1 1 calc R U . . .
H7C H 0.724665 1.066321 0.202870 0.191 Uiso 1 1 calc R U . . .
C8 C 0.7877(8) 0.8451(13) 0.2914(10) 0.122(3) Uani 1 1 d . . . . .
H8A H 0.823051 0.906091 0.409665 0.183 Uiso 1 1 calc R U . . .
H8B H 0.877820 0.892375 0.258003 0.183 Uiso 1 1 calc R U . . .
H8C H 0.776974 0.729799 0.257602 0.183 Uiso 1 1 calc 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'
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
S2 Ni1 S2 180.0 . 2 ?
S2 Ni1 S1 91.96(4) . . ?
S2 Ni1 S1 88.04(4) 2 . ?
S2 Ni1 S1 88.04(4) . 2 ?
S2 Ni1 S1 91.96(4) 2 2 ?
S1 Ni1 S1 180.0 . 2 ?
C2 S1 Ni1 103.27(13) . . ?
C3 S2 Ni1 103.45(15) . . ?
C8 N3 C6 111.9(5) . . ?
C8 N3 C5 111.1(4) . . ?
C6 N3 C5 109.7(4) . . ?
C8 N3 C7 109.9(5) . . ?
C6 N3 C7 103.5(5) . . ?
C5 N3 C7 110.5(5) . . ?
N1 C1 C2 178.1(5) . . ?
C3 C2 C1 122.1(4) . . ?
C3 C2 S1 119.9(3) . . ?
C1 C2 S1 118.0(3) . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 S2 121.4(3) . . ?
C4 C3 S2 118.4(3) . . ?
N2 C4 C3 178.0(5) . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
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 S2 2.1695(11) . ?
Ni1 S2 2.1695(11) 2 ?
Ni1 S1 2.1762(9) . ?
Ni1 S1 2.1762(9) 2 ?
S1 C2 1.742(4) . ?
S2 C3 1.723(4) . ?
N1 C1 1.139(5) . ?
N2 C4 1.146(6) . ?
N3 C8 1.456(6) . ?
N3 C6 1.465(6) . ?
N3 C5 1.475(6) . ?
N3 C7 1.510(8) . ?
C1 C2 1.423(5) . ?
C2 C3 1.358(6) . ?
C3 C4 1.427(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
