A hybrid hydrochromic molecular crystal applicable to invisible ink with high reversibility
Huang, Yao; Zhang, Tie; Chu, Lu-Lu; Zhang, Yi; Ge, Jia-Zhen; Fu, Da-Wei; New Journal of Chemistry 45 (2021) 21006–21010; doi:10.1039/D1NJ04470B

data_7061027
_publ_section_title
;
 A hybrid hydrochromic molecular crystal applicable to invisible ink with
 high reversibility
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21006
_journal_page_last               21010
_journal_paper_doi               10.1039/D1NJ04470B
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C2 H2 Mn0.5 N2 O S2, C4 H10 N'
_chemical_formula_sum            'C6 H12 Mn0.5 N3 O S2'
_chemical_formula_weight         233.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-10
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2018.02.02 svn.r3482 for Rigaku Oxford Diffraction, GUI svn.r5381)
;
_audit_update_record
;
2021-03-03 deposited with the CCDC.	2021-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.428(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1894(3)
_cell_length_b                   7.3513(1)
_cell_length_c                   13.8269(3)
_cell_measurement_reflns_used    16878
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.4660
_cell_measurement_theta_min      1.9870
_cell_volume                     1058.74(4)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.8937
_diffrn_measured_fraction_theta_max 0.8937
_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    -69.00  28.00   0.50    0.10    --    7.97 -28.00 -59.00  194
  2  \w    -66.00 -10.00   0.50    0.10    --    7.97 -57.00-120.00  112
  3  \w     -7.00  28.00   0.50    0.10    --    7.97 -57.00-120.00   70
  4  \w     14.00  85.00   0.50    0.10    --    7.97  28.00 102.00  142
  5  \w    -74.00 -46.00   0.50    0.10    --   -8.51 -28.00 -59.00   56
  6  \w    -16.00  29.00   0.50    0.10    --   -8.51 -99.00-120.00   90
  7  \w    -17.00  29.00   0.50    0.10    --   -8.51 -99.00 -30.00   92
  8  \w    -18.00  23.00   0.50    0.10    --   -8.51 -99.00  60.00   82
  9  \w    -83.00  10.00   0.50    0.10    --   -8.51 -38.00 150.00  186
 10  \w    -55.00  -6.00   0.50    0.10    --   -8.51 114.00 -53.37   98
 11  \w    -54.00 -29.00   0.50    0.10    --   -8.51 113.00-162.57   50
 12  \w     13.00  67.00   0.50    0.10    --   -8.51  38.00-180.00  108
 13  \w    -28.00  -3.00   0.50    0.10    --   -8.51  28.00 102.00   50
 14  \w      1.00  61.00   0.50    0.10    --   -8.51  28.00 102.00  120
 15  \w    -28.00  10.00   0.50    0.10    --   -8.51  38.00-180.00   76
 16  \w      5.00  48.00   0.50    0.10    --    7.97-103.00  73.85   86
 17  \w    -17.00   9.00   0.50    0.10    --    7.97 -99.00 120.00   52
 18  \w     -7.00  45.00   0.50    0.10    --    7.97 -99.00 150.00  104
 19  \w     20.00  45.00   0.50    0.10    --    7.97 -99.00 120.00   50
 20  \w      7.00  48.00   0.50    0.10    --    7.97-103.00 -16.49   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0610684000
_diffrn_orient_matrix_UB_12      -0.0427100000
_diffrn_orient_matrix_UB_13      0.0186001000
_diffrn_orient_matrix_UB_21      -0.0288369000
_diffrn_orient_matrix_UB_22      -0.0820395000
_diffrn_orient_matrix_UB_23      0.0075033000
_diffrn_orient_matrix_UB_31      -0.0087953000
_diffrn_orient_matrix_UB_32      -0.0274615000
_diffrn_orient_matrix_UB_33      -0.0513235000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29973
_diffrn_reflns_theta_full        30.5833
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79460
_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_density_diffrn    1.4666
_exptl_crystal_F_000             486.0
_refine_diff_density_max         0.5911
_refine_diff_density_min         -0.9301
_refine_diff_density_rms         0.1538
_refine_ls_d_res_high            0.6985
_refine_ls_d_res_low             10.4160
_refine_ls_goodness_of_fit_ref   1.0355
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    17
_refine_ls_number_parameters     118
_refine_ls_number_reflns         3252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0355
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.1914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2530
_reflns_number_total             3252
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj04470b2.cif
_cod_data_source_block           hy1110_198k
_cod_depositor_comments          'Adding full bibliography for 7061027.cif.'
_cod_original_cell_volume        1058.74(5)
_cod_original_sg_symbol_H-M      'P  21/c '
_cod_database_code               7061027
_chemical_oxdiff_formula         'C1 H1 N1 O1 S1 Cl1 Mn1'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O8(H8a,H8b)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C9(H9a,H9b)
2.c Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C12(H12a,H12b,H12c)
;
_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 1.234
_oxdiff_exptl_absorpt_empirical_full_min 0.781