#------------------------------------------------------------------------------
#$Date: 2022-11-10 00:57:36 +0200 (Thu, 10 Nov 2022) $
#$Revision: 279159 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/09/7130976.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_7130976
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(C64 H144 N16 S16 Sn4 Zn8)'
_chemical_formula_sum            'C16 H36 N4 S4 Sn Zn2'
_chemical_formula_weight         662.16
_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     direct
_audit_creation_date             2022-09-23
_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                   13.44118(7)
_cell_length_b                   13.44118(7)
_cell_length_c                   14.28207(11)
_cell_measurement_reflns_used    3104
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3450
_cell_measurement_theta_min      4.6630
_cell_volume                     2580.27(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  30.00   0.50    0.50    --   -2.20  73.00 121.00   58
  2  ω     76.00 135.00   0.50    0.50    --  106.30 -65.00-140.00  118
  3  ω     30.00  55.00   0.50    0.50    --  106.30 -65.00-140.00   50
  4  ω    -39.00  31.00   0.50    0.50    --   -2.20 -82.00 -60.00  140
  5  ω     86.00 194.00   0.50    0.50    --  106.30  38.00 -30.00  216
  6  ω     80.00 118.00   0.50    0.50    --  106.30  57.00-120.00   76
  7  ω    165.00 191.00   0.50    0.50    --  106.30  57.00-120.00   52
  8  ω    115.00 140.00   0.50    0.50    --  106.30  73.00 121.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0992982000
_diffrn_orient_matrix_UB_12      0.0265716000
_diffrn_orient_matrix_UB_13      -0.0476635000
_diffrn_orient_matrix_UB_21      0.0178350000
_diffrn_orient_matrix_UB_22      -0.0820467000
_diffrn_orient_matrix_UB_23      -0.0733880000
_diffrn_orient_matrix_UB_31      -0.0542865000
_diffrn_orient_matrix_UB_32      -0.0755026000
_diffrn_orient_matrix_UB_33      0.0631366000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3389
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.925
_diffrn_reflns_theta_min         6.587
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    12.900
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Flack x determined using 518 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         1276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0266
_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)+(0.0516P)²+3.5447P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.699
_reflns_Friedel_fraction_full    0.913
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                1275
_reflns_number_total             1276
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc05407h2.cif
_cod_data_source_block           1-me-cu
_cod_database_code               7130976
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Zn Sn S N C'
_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.
;
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.817
_oxdiff_exptl_absorpt_empirical_full_min 0.794
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y+1/2, -z+1/4'
'-x, y+1/2, -z+1/4'
'-y, -x+1/2, z+1/4'
'y, x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, y+1, -z+3/4'
'-y+1/2, -x+1, z+3/4'
'y+1/2, x+1, z+3/4'
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 0.000000 0.000000 0.000000 0.01289(18) Uani 1 4 d S T P . .
Zn1 Zn 0.00610(7) 0.250000 0.125000 0.0156(2) Uani 1 2 d S T P . .
S1 S -0.09079(8) 0.11334(8) 0.09611(8) 0.0159(3) Uani 1 1 d . . . . .
N1 N 0.1207(3) 0.2899(3) 0.0343(3) 0.0203(8) Uani 1 1 d . . . . .
H1 H 0.128760 0.234672 -0.009782 0.024 Uiso 1 1 calc R . . . .
C1 C 0.1022(4) 0.3799(4) -0.0224(4) 0.0264(11) Uani 1 1 d . . . . .
H1A H 0.041019 0.372235 -0.056329 0.040 Uiso 1 1 calc GR . . . .
H1B H 0.155981 0.389139 -0.065784 0.040 Uiso 1 1 calc GR . . . .
H1C H 0.097590 0.436793 0.017984 0.040 Uiso 1 1 calc GR . . . .
C2 C 0.2125(3) 0.2939(3) 0.0907(4) 0.0227(11) Uani 1 1 d . . . . .
H2 H 0.211175 0.355500 0.127445 0.027 Uiso 1 1 calc R . . . .
C3 C 0.3061(4) 0.2950(4) 0.0312(5) 0.0330(13) Uani 1 1 d . . . . .
H3A H 0.306205 0.353906 -0.008049 0.040 Uiso 1 1 calc R . . . .
H3B H 0.306456 0.237159 -0.009487 0.040 Uiso 1 1 calc R . . . .
C4 C 0.4010(4) 0.2943(4) 0.0927(6) 0.0437(16) Uani 1 1 d . . . . .
H4A H 0.459410 0.292054 0.052859 0.052 Uiso 1 1 calc R . . . .
H4B H 0.403861 0.355020 0.129311 0.052 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn 0.0259 5.4591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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 109.32(3) . 4 ?
S1 Sn1 S1 109.33(3) 4 3 ?
S1 Sn1 S1 109.33(3) . 2 ?
S1 Sn1 S1 109.33(3) 2 3 ?
S1 Sn1 S1 109.76(5) . 3 ?
S1 Sn1 S1 109.76(5) 4 2 ?
S1 Zn1 S1 110.65(6) 5 . ?
N1 Zn1 S1 121.03(11) 5 5 ?
N1 Zn1 S1 109.03(11) . 5 ?
N1 Zn1 S1 109.03(11) 5 . ?
N1 Zn1 S1 121.03(11) . . ?
N1 Zn1 N1 84.6(2) 5 . ?
Zn1 S1 Sn1 108.96(4) . . ?
C1 N1 Zn1 115.3(3) . . ?
C2 N1 Zn1 106.8(3) . . ?
C2 N1 C1 114.2(4) . . ?
N1 C2 C2 108.7(3) . 5 ?
N1 C2 C3 112.8(5) . . ?
C3 C2 C2 111.4(4) . 5 ?
C2 C3 C4 111.4(5) . . ?
C4 C4 C3 110.6(4) 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
Sn1 S1 2.3863(10) . ?
Sn1 S1 2.3863(10) 4 ?
Sn1 S1 2.3863(10) 3 ?
Sn1 S1 2.3863(10) 2 ?
Zn1 S1 2.2892(11) . ?
Zn1 S1 2.2892(11) 5 ?
Zn1 N1 2.083(4) . ?
Zn1 N1 2.083(4) 5 ?
N1 C1 1.477(6) . ?
N1 C2 1.474(6) . ?
C2 C2 1.535(10) 5 ?
C2 C3 1.519(7) . ?
C3 C4 1.548(9) . ?
C4 C4 1.508(14) 5 ?
