Stimuli-responsive and chemically tunable organic microcrystal laser switch
Fu, Hongbing; Cai, Xin; Xu, Zhenzhen; Zheng, Xiaolin; Ran, Chenhui; Liu, Peng; He, Xianxiong; Jin, Xue; Liao, Qing; Chemical Communications  (2018) –; doi:10.1039/C8CC08298G

data_7122740
_publ_section_title
;
 Stimuli-responsive and chemically tunable organic microcrystal laser
 switch
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08298G
_journal_year                    2018
_chemical_formula_moiety         'C48 H52 N2 O4'
_chemical_formula_sum            'C48 H52 N2 O4'
_chemical_formula_weight         720.91
_chemical_name_common            5-PDA
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc1zy413
_audit_creation_date             2018-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-05-25 deposited with the CCDC.
2018-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                81.489(9)
_cell_angle_beta                 88.641(12)
_cell_angle_gamma                79.847(12)
_cell_formula_units_Z            1
_cell_length_a                   5.9659(10)
_cell_length_b                   8.1499(9)
_cell_length_c                   20.8277(19)
_cell_measurement_reflns_used    1411
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.1040
_cell_measurement_theta_min      5.5370
_cell_volume                     985.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.943
_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    -11.00  28.00   1.00    5.00    --  -40.73  57.00-120.00   39
  2  \w    -65.00 -17.00   1.00    5.00    --  -40.73  57.00-120.00   48
  3  \w     35.00  66.00   1.00    5.00    --   40.73 -99.00 -30.00   31
  4  \w     27.00  56.00   1.00    5.00    --   40.73 -99.00 -60.00   29
  5  \w     85.00 117.00   1.00    8.61    --  106.95-125.00 -60.00   32
  6  \w     63.00  92.00   1.00   10.00    --  106.95 -45.00-150.00   29
  7  \w     49.00  81.00   1.00   10.00    --  106.95-125.00 -60.00   32
  8  \w     28.00  60.00   1.00   10.00    --  106.95 -95.00  90.00   32
  9  \w     71.00 101.00   1.00   10.00    --  106.95 -95.00  90.00   30
 10  \w     77.00 135.00   1.00   10.00    --  106.95 -61.00  90.00   58
 11  \w    101.00 151.00   1.00   10.00    --  106.95  15.00 150.00   50
 12  \w    152.00 178.00   1.00   10.00    --  106.95  15.00 150.00   26
 13  \w    127.00 161.00   1.00   10.00    --  106.95 107.00 103.00   34
 14  \w     97.00 176.00   1.00   10.00    --  106.95 125.00 150.00   79
 15  \w    122.00 152.00   1.00   10.00    --  106.95 125.00 -90.00   30
 16  \w    131.00 175.00   1.00   10.00    --  106.95  45.00-120.00   44
 17  \w     88.00 129.00   1.00   10.00    --  106.95  45.00-120.00   41
 18  \w   -110.00 -30.00   1.00   10.00    --  -40.73 -57.00  90.00   80
 19  \w      7.00  32.00   1.00   10.00    --  -41.84  38.00-150.00   25
 20  \w    -52.00 -26.00   1.00   10.00    --  -41.84  38.00-150.00   26
 21  \w    -99.00 -73.00   1.00   10.00    --  -41.84 -38.00  30.00   26
 22  \w     58.00 114.00   1.00   10.00    --   42.31  57.00 -30.00   56
 23  \w     93.00 131.00   1.00   10.00    --   42.31 178.00  90.00   38
 24  \w     20.00  51.00   1.00   10.00    --   42.31  57.00 -30.00   31
 25  \w    143.00 174.00   1.00    9.89    --  106.95  61.00 -60.00   31
 26  \w     97.00 128.00   1.00    9.89    --  106.95 125.00  30.00   31
 27  \w     51.00  91.00   1.00    9.89    --  106.95 -45.00   0.00   40
 28  \w    103.00 141.00   1.00    9.89    --  106.95 118.00 124.00   38
 29  \w     82.00 122.00   1.00    9.89    --  106.95  45.00-150.00   40
 30  \w    138.00 164.00   1.00    9.89    --  106.95  45.00-150.00   26
 31  \w     36.00  65.00   1.00    9.89    --  106.95 -95.00 120.00   29
 32  \w     84.00 109.00   1.00    9.89    --  106.95 -95.00 120.00   25
 33  \w     70.00 108.00   1.00    9.89    --  106.95 -77.00-180.00   38
 34  \w     55.00  87.00   1.00    9.89    --  106.95 -77.00 -60.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2287988000
_diffrn_orient_matrix_UB_12      -0.0626292000
_diffrn_orient_matrix_UB_13      0.0111776000
_diffrn_orient_matrix_UB_21      0.0179824000
_diffrn_orient_matrix_UB_22      0.0059987000
_diffrn_orient_matrix_UB_23      0.0732530000
_diffrn_orient_matrix_UB_31      -0.1270735000
_diffrn_orient_matrix_UB_32      0.1836408000
_diffrn_orient_matrix_UB_33      -0.0101358000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7029
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.593
_diffrn_reflns_theta_min         2.145
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             386
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMSO'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.0923
_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^)+(0.1430P)^2^+0.9025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2725
_refine_ls_wR_factor_ref         0.3050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2362
_reflns_number_total             3764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08298g2.cif
_cod_data_source_block           exp_1406
_cod_database_code               7122740
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.921
_reflns_odcompleteness_completeness 98.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C7(H7), C18(H18), C10(H10), C13(H13), C16(H16), C6(H6), C8(H8),
 C3(H3), C2(H2), C5(H5)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C23(H23A,H23B,H23C)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.392
_oxdiff_exptl_absorpt_empirical_full_min 0.679