A single-crystal-to-single-crystal transformation affording photochromic 3D MORF crystals
Yang, Xue; Giorgi, Michel; Karoui, Hakim; Gigmes, Didier; Hornebecq, Virginie; Ouari, Olivier; Kermagoret, Anthony; Bardelang, David; Chemical Communications  (2019) –; doi:10.1039/C9CC07121K

data_7124369
_publ_section_title
;
 A single-crystal-to-single-crystal transformation affording photochromic
 3D MORF crystals
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07121K
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C12 H8 N O2 Zn0.25, C21 H20 N14 O7, 0.5(H2 O), 0.5(N O2)'
_chemical_formula_sum            'C33 H29 N15.5 O10.5 Zn0.25'
_chemical_formula_weight         827.06
_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'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2019-09-02 deposited with the CCDC.    2019-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   32.6797(2)
_cell_length_b                   32.6797(2)
_cell_length_c                   13.5625(2)
_cell_measurement_reflns_used    14743
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      70.9080
_cell_measurement_theta_min      4.2570
_cell_volume                     14484.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_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    -76.00 -14.00   1.00   10.00    --  -41.07 -57.00 -90.00   62
  2  \w   -113.00 -81.00   1.00   10.00    --  -41.07 -77.00-150.00   32
  3  \w    -41.00  -8.00   1.00   10.00    --  -41.07 -77.00-150.00   33
  4  \w      1.00  63.00   1.00   10.00    --   41.07 -99.00  60.00   62
  5  \w     62.00  87.00   1.00   10.00    --   41.07-125.00-180.00   25
  6  \w     72.00  98.00   1.00   30.00    --  101.41  61.00-120.00   26
  7  \w     69.00 178.00   1.00   30.00    --  101.41  77.00-150.00  109
  8  \w     95.00 172.00   1.00   30.00    --  101.41 125.00   0.00   77
  9  \w     69.00  95.00   1.00   30.00    --  101.41  77.00-120.00   26
 10  \w     72.00 112.00   1.00   30.00    --  101.41  61.00-150.00   40
 11  \w    149.00 174.00   1.00   30.00    --  101.41  45.00 -90.00   25
 12  \w     72.00 111.00   1.00   30.00    --  101.41  61.00-180.00   39
 13  \w     70.00 120.00   1.00   30.00    --  101.41  77.00-180.00   50
 14  \w    101.00 177.00   1.00   30.00    --  101.41 113.00-122.00   76
 15  \w     77.00 104.00   1.00   30.00    --  101.41  45.00 -90.00   27
 16  \w     71.00  96.00   1.00   30.00    --  101.41  74.00-154.51   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0453323000
_diffrn_orient_matrix_UB_12      -0.0108882000
_diffrn_orient_matrix_UB_13      0.0168210000
_diffrn_orient_matrix_UB_21      -0.0094222000
_diffrn_orient_matrix_UB_22      0.0452841000
_diffrn_orient_matrix_UB_23      0.0220326000
_diffrn_orient_matrix_UB_31      -0.0087922000
_diffrn_orient_matrix_UB_32      0.0073918000
_diffrn_orient_matrix_UB_33      -0.1101466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32827
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.082
_diffrn_reflns_theta_min         3.528
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       plate
_exptl_crystal_F_000             6832
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 2640 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         6829
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0507
_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^)+(0.1037P)^2^+3.5351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                6301
_reflns_number_total             6829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07121k2.cif
_cod_data_source_block           diac13amb
_cod_original_cell_volume        14484.2(3)
_cod_original_formula_sum        'C33 H29 N15.50 O10.50 Zn0.25'
_cod_database_code               7124369
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.695
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N16-O11
 1.25 with sigma of 0.001
3. Others
 Fixed Sof: O10(0.5) H10C(0.5) H10D(0.5) O11(0.5)
4.a Riding coordinates:
 O10(H10C,H10D)
4.b Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C20(H20)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C15(H15A,H15B),
 C19(H19A,H19B), C22(H22A,H22B)
4.d Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34)
;
_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 1.543
_oxdiff_exptl_absorpt_empirical_full_min 0.626