#------------------------------------------------------------------------------
#$Date: 2022-11-09 23:57:36 +0100 (Wed 09 de Nov de 2022) $
#$Revision: 279159 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/09/7130975.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_7130975
loop_
_publ_author_name
'Lin-Mei, Zhang'
'Kong, Yinan'
'Zhou, Rui'
'Yuan, Shang-Fu'
'Wu, Tao'
_publ_section_title
;
 X-ray photochromism of chalcogenide frameworks linked with metal-amine
 chelates
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC05407H
_journal_year                    2022
_chemical_formula_moiety         '0.25(C48 H112 N16 S16 Sn4 Zn8)'
_chemical_formula_sum            'C12 H28 N4 S4 Sn Zn2'
_chemical_formula_weight         606.05
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-02 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0687(4)
_cell_length_b                   10.0687(4)
_cell_length_c                   20.8088(7)
_cell_measurement_reflns_used    7701
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.47
_cell_volume                     2109.57(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      119.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13160
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_min         3.467
_exptl_absorpt_coefficient_mu    3.829
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1506 before and 0.0804 after correction.
The Ratio of minimum to maximum transmission is 0.7955.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_colour_primary    pale-yellow
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0254
_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)+(0.0089P)²+13.3008P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1160
_reflns_number_total             1225
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc05407h2.cif
_cod_data_source_block           a
_cod_original_cell_volume        2109.57(18)
_cod_database_code               7130975
_shelx_shelxl_version_number     2014/7
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.98(3)
 0.02(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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
Sn1 Sn -1.0000 -1.0000 -0.5000 0.01158(17) Uani 1 4 d S T P . .
Zn1 Zn -1.2500 -1.02651(8) -0.6250 0.0144(2) Uani 1 2 d S T P . .
S1 S -1.11173(14) -1.15974(13) -0.56576(6) 0.0138(3) Uani 1 1 d . . . . .
N1 N -1.3438(5) -0.8711(5) -0.5756(2) 0.0164(10) Uani 1 1 d . . . . .
H1A H -1.4299 -0.8639 -0.5883 0.020 Uiso 1 1 calc R . . . .
H1B H -1.3422 -0.8867 -0.5325 0.020 Uiso 1 1 calc R . . . .
C1 C -1.2708(7) -0.7479(6) -0.5907(3) 0.0320(15) Uani 1 1 d . . . . .
H1 H -1.1878 -0.7486 -0.5642 0.038 Uiso 1 1 calc R . . . .
C2 C -1.3469(7) -0.6220(6) -0.5729(3) 0.0235(13) Uani 1 1 d . . . . .
H2A H -1.4342 -0.6226 -0.5948 0.028 Uiso 1 1 calc R . . . .
H2B H -1.3631 -0.6210 -0.5260 0.028 Uiso 1 1 calc R . . . .
C3 C -1.2719(9) -0.4986(8) -0.5917(3) 0.045(2) Uani 1 1 d . . . . .
H3A H -1.3296 -0.4204 -0.5845 0.054 Uiso 1 1 calc R . . . .
H3B H -1.1933 -0.4894 -0.5635 0.054 Uiso 1 1 calc R . . . .
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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
S1 Sn1 S1 109.09(3) 4_354 2_335 ?
S1 Sn1 S1 109.09(3) 2_335 3_534 ?
S1 Sn1 S1 109.09(3) 3_534 . ?
S1 Sn1 S1 110.23(6) 2_335 . ?
S1 Sn1 S1 110.23(6) 4_354 3_534 ?
S1 Sn1 S1 109.09(3) 4_354 . ?
S1 Zn1 S1 108.39(8) 5_253 . ?
N1 Zn1 S1 116.51(13) . . ?
N1 Zn1 S1 116.51(13) 5_253 5_253 ?
N1 Zn1 S1 115.27(14) . 5_253 ?
N1 Zn1 S1 115.27(14) 5_253 . ?
N1 Zn1 N1 83.5(3) . 5_253 ?
Zn1 S1 Sn1 101.52(5) . . ?
C1 N1 Zn1 107.4(4) . . ?
N1 C1 C1 110.1(5) . 5_253 ?
N1 C1 C2 113.4(5) . . ?
C1 C1 C2 111.9(5) 5_253 . ?
C3 C2 C1 111.8(6) . . ?
C3 C3 C2 113.6(5) 5_253 . ?
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
Sn1 S1 2.3927(13) 4_354 ?
Sn1 S1 2.3927(13) . ?
Sn1 S1 2.3927(13) 2_335 ?
Sn1 S1 2.3927(13) 3_534 ?
Zn1 S1 2.2928(14) . ?
Zn1 S1 2.2928(14) 5_253 ?
Zn1 N1 2.097(5) . ?
Zn1 N1 2.097(5) 5_253 ?
N1 C1 1.475(8) . ?
C1 C1 1.489(13) 5_253 ?
C1 C2 1.526(9) . ?
C2 C3 1.506(10) . ?
C3 C3 1.453(13) 5_253 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.98(3)
2 0.02(3)
