Fluorescence response of cruciform D–π–A–π–D phenothiazine derivatives to mechanical force
Zhang, Tong; Zhang, Chunyu; Li, Xiaoting; Liang, Meng; Bian, Weixiao; Zhang, Yan; Wang, Kunpeng; Xue, Pengchong; CrystEngComm 21 (2019) 4192–; doi:10.1039/C9CE00568D

data_7232936
_publ_section_title
;
 Fluorescence response of cruciform D--\p--A--\p--D phenothiazine
 derivatives to mechanical force
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              4192
_journal_paper_doi               10.1039/C9CE00568D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C48 H48 N2 O4 S2'
_chemical_formula_sum            'C48 H48 N2 O4 S2'
_chemical_formula_weight         781.00
_chemical_name_systematic        EPTD
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-03-27 deposited with the CCDC.    2019-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.503(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7972(4)
_cell_length_b                   9.6008(5)
_cell_length_c                   24.5152(17)
_cell_measurement_reflns_used    3909
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.5200
_cell_measurement_theta_min      2.2640
_cell_volume                     2042.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5479
_diffrn_detector_type            AtlasS2
_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      1.00  41.50   0.75    5.84    --   11.08 -77.00  60.00   54
  2  \w     34.00  89.50   0.75    5.84    --   11.08-178.00  90.00   74
  3  \w     -8.00  76.00   0.75    5.84    --   11.08  38.00-120.00  112
  4  \w    -18.00  25.50   0.75    5.84    --  -11.24 -99.00-120.00   58
;
_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      -0.0034471000
_diffrn_orient_matrix_UB_12      0.0328712000
_diffrn_orient_matrix_UB_13      -0.0261105000
_diffrn_orient_matrix_UB_21      -0.0286478000
_diffrn_orient_matrix_UB_22      -0.0624147000
_diffrn_orient_matrix_UB_23      -0.0133822000
_diffrn_orient_matrix_UB_31      -0.0764302000
_diffrn_orient_matrix_UB_32      0.0218824000
_diffrn_orient_matrix_UB_33      0.0010423000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10301
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.282
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0425P)^2^+1.3720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2787
_reflns_number_total             3610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00568d2.cif
_cod_data_source_block           a180504d
_cod_depositor_comments
'Adding full bibliography for 7232936--7232938.cif.'
_cod_original_cell_volume        2042.17(19)
_cod_database_code               7232936
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups
2. Restrained distances
 O2-C22 = O2A-C22
 1.15 with sigma of 0.01
 O1A-C22 = O1-C22
 1.35 with sigma of 0.01
 O1-C23 = O1A-C23A
 1.48 with sigma of 0.01
 C23-C24 = C23A-C24A
 1.56 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O2A) = Uanis(O2)
Uanis(O1) = Uanis(O1A)
Uanis(C23) = Uanis(C23A)
Uanis(C24A) = Uanis(C24)
4. Others
 Sof(O1A)=Sof(O2A)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C23(H23A,H23B), C23A(H23C,H23D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C17(H17),
 C18(H18), C20(H20)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2018-05-04
_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 1.626
_oxdiff_exptl_absorpt_empirical_full_min 0.607