X-ray photochromism of chalcogenide frameworks linked with metal-amine chelates
Lin-Mei, Zhang; Kong, Yinan; Zhou, Rui; Yuan, Shang-Fu; Wu, Tao; Chemical Communications  (2022) –; doi:10.1039/D2CC05407H

data_7130976
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  30.00   0.50    0.50    --   -2.20  73.00 121.00   58
  2  \w     76.00 135.00   0.50    0.50    --  106.30 -65.00-140.00  118
  3  \w     30.00  55.00   0.50    0.50    --  106.30 -65.00-140.00   50
  4  \w    -39.00  31.00   0.50    0.50    --   -2.20 -82.00 -60.00  140
  5  \w     86.00 194.00   0.50    0.50    --  106.30  38.00 -30.00  216
  6  \w     80.00 118.00   0.50    0.50    --  106.30  57.00-120.00   76
  7  \w    165.00 191.00   0.50    0.50    --  106.30  57.00-120.00   52
  8  \w    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       '\w 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/[\s^2^(Fo^2^)+(0.0516P)^2^+3.5447P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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'
_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)
;
_shelx_res_checksum              36525
_shelx_hkl_checksum              68501
_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