Photochromic Metal-Organic Framework for High-Resolution Inkless and Erasable Printing.
Li, Wen-Bin; Chen, Xiong-Hai; Chen, Jia-Zhe; Huang, Rong; Ye, Jia-Wen; Chen, Ling; Wang, Hai-Ping; Yang, Tao; Tang, Liu-Yan; Bai, Jie; Mo, Zong-Wen; Chen, Xiao-Ming; ACS applied materials & interfaces 14 (2022) 8458–8463; doi:10.1021/acsami.1c23512

data_4519326
_publ_section_title
;
 Photochromic Metal-Organic Framework for High-Resolution Inkless and
 Erasable Printing.
;
_journal_issue                   6
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              8458
_journal_page_last               8463
_journal_paper_doi               10.1021/acsami.1c23512
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C49 H28 Ca3 N4 O21, 3(H2 O)'
_chemical_formula_sum            'C49 H34 Ca3 N4 O24'
_chemical_formula_weight         1183.04
_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   mixed
_audit_creation_date             2022-01-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                73.2120(10)
_cell_angle_beta                 86.2070(10)
_cell_angle_gamma                72.1550(10)
_cell_formula_units_Z            2
_cell_length_a                   10.03920(10)
_cell_length_b                   15.8473(2)
_cell_length_c                   18.4586(2)
_cell_measurement_reflns_used    22613
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.7710
_cell_measurement_theta_min      4.4420
_cell_volume                     2675.43(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -68.00  10.00   0.50    0.12    --  -48.57  73.00   9.00  156
  2  \w    -24.00  21.00   0.50    0.12    --  -48.57  19.00 -60.00   90
  3  \w    -26.00  23.00   0.50    0.12    --  -48.57  19.00   0.00   98
  4  \w    -42.00 -13.00   0.50    0.48    --  -86.25  38.00 -30.00   58
  5  \w    -49.00 -24.00   0.50    0.48    --  -86.25  73.00   9.00   50
  6  \w    -84.00 -13.00   0.50    0.12    --  -48.57 125.00  30.00  142
  7  \w    -43.00 -14.00   0.50    0.48    --  -86.25  38.00 150.00   58
  8  \w    -98.00 -73.00   0.50    0.48    --  -86.25 -38.00  90.00   50
  9  \w   -157.00-103.00   0.50    0.48    --  -86.25 -38.00  90.00  108
 10  \w   -120.00 -28.00   0.50    0.12    --  -48.57 -73.00-120.00  184
 11  \w    -43.00 -14.00   0.50    0.48    --  -86.25  38.00-150.00   58
 12  \w    -43.00 -13.00   0.50    0.48    --  -86.25  38.00-180.00   60
 13  \w    -45.00 -17.00   0.50    0.48    --  -86.25  57.00-150.00   56
 14  \w   -146.00 -83.00   0.50    0.48    --  -86.25 -73.00-120.00  126
 15  \w   -111.00 -83.00   0.50    0.12    --  -48.57-125.00-180.00   56
 16  \w    -15.00  10.00   0.50    0.12    --   48.57 -73.00-120.00   50
 17  \w     18.00  50.00   0.50    0.12    --   48.57 -73.00-120.00   64
 18  \w     35.00  92.00   0.50    0.48    --  107.75 -73.00-120.00  114
 19  \w     66.00 112.00   0.50    0.48    --  107.75-125.00-150.00   92
 20  \w     54.00 104.00   0.50    0.48    --  107.75-125.00 -30.00  100
 21  \w     80.00 112.00   0.50    0.48    --  107.75-125.00  60.00   64
 22  \w     58.00 103.00   0.50    0.48    --  107.75-125.00   0.00   90
 23  \w     43.00 108.00   0.50    0.48    --  107.75-112.00  68.09  130
 24  \w     40.00  95.00   0.50    0.48    --  107.75 -99.00 150.00  110
 25  \w     35.00  66.00   0.50    0.48    --  107.75-125.00  60.00   62
 26  \w     39.00 112.00   0.50    0.48    --  107.75-125.00  30.00  146
 27  \w     38.00 103.00   0.50    0.48    --  107.75 -99.00-120.00  130
 28  \w     40.00  65.00   0.50    0.48    --  107.75 -99.00-180.00   50
 29  \w     39.00  65.00   0.50    0.48    --  107.75-125.00-150.00   52
 30  \w     46.00 112.00   0.50    0.48    --  107.75-125.00-120.00  132
 31  \w     35.00  60.00   0.50    0.48    --  107.75 -57.00   0.00   50
 32  \w     39.00  64.00   0.50    0.48    --  107.75 -57.00 -60.00   50
 33  \w     46.00  77.00   0.50    0.48    --  107.75   0.00-120.00   62
 34  \w     90.00 116.00   0.50    0.48    --  107.75   0.00-120.00   52
 35  \w    113.00 167.00   0.50    0.48    --  107.75  38.00 -90.00  108
 36  \w    152.00 177.00   0.50    0.48    --  107.75   0.00-120.00   50
 37  \w    123.00 176.00   0.50    0.48    --  107.75  19.00 -60.00  106
 38  \w    100.00 178.00   0.50    0.48    --  107.75  38.00 -30.00  156
 39  \w     97.00 163.00   0.50    0.48    --  107.75  73.00   9.00  132
 40  \w     62.00  87.00   0.50    0.12    --   48.57  73.00   9.00   50
 41  \w     36.00  65.00   0.50    0.48    --  107.75 -57.00  30.00   58
 42  \w     37.00 100.00   0.50    0.48    --  107.75 -99.00 120.00  126
 43  \w     37.00 112.00   0.50    0.48    --  107.75-125.00 120.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.5478
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34310
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.109
_diffrn_reflns_theta_max         67.109
_diffrn_reflns_theta_min         4.481
_exptl_absorpt_coefficient_mu    3.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         9426
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+2.3740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8633
_reflns_number_total             9426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c23512_si_002.cif
_cod_data_source_block           1
_cod_database_code               4519326
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.992
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O19-H19A = O19-H19B
 0.87 with sigma of 0.02
 H19A-H19B
 1.38 with sigma of 0.04
 Ca02-H19A \\sim Ca02-H19B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O2B(0.5) O2A(0.5)
5.a Free rotating group:
 O2(H2A,H2B)
5.b Rotating group:
 O20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C30(H30), C3(H3), C38(H38), C33(H33), C24(H24), C7(H7), C5(H5),
 C36(H36), C18(H18), C19(H19), C13(H13), C42(H42), C45(H45), C12(H12)
5.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61048
_shelx_hkl_checksum              97587
_shelx_fab_checksum              94552
_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
;