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_7232938
_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         'C44 H40 N2 O4 S2'
_chemical_formula_sum            'C44 H40 N2 O4 S2'
_chemical_formula_weight         724.90
_chemical_name_systematic        EPTD-Y
_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
_audit_creation_date             2018-05-04
_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                102.649(4)
_cell_angle_beta                 93.485(4)
_cell_angle_gamma                99.072(5)
_cell_formula_units_Z            2
_cell_length_a                   11.2305(6)
_cell_length_b                   11.8596(6)
_cell_length_c                   14.1250(7)
_cell_measurement_reflns_used    4769
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.3950
_cell_measurement_theta_min      2.3340
_cell_volume                     1803.79(17)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_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    -16.00  84.00   1.00    4.20    --   10.93  57.00  30.00  100
  2  \w    -29.00  -4.00   1.00    4.20    --   10.93  97.00-172.37   25
  3  \w    -56.00  35.00   1.00    4.20    --   10.93 -57.00-120.00   91
  4  \w    -76.00  17.00   1.00    4.20    --  -11.01 -57.00  90.00   93
;
_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      -0.0470806000
_diffrn_orient_matrix_UB_12      0.0131426000
_diffrn_orient_matrix_UB_13      0.0296096000
_diffrn_orient_matrix_UB_21      0.0205220000
_diffrn_orient_matrix_UB_22      0.0608308000
_diffrn_orient_matrix_UB_23      0.0045695000
_diffrn_orient_matrix_UB_31      -0.0386437000
_diffrn_orient_matrix_UB_32      -0.0018881000
_diffrn_orient_matrix_UB_33      -0.0421572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13018
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.485
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79644
_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    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6355
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+1.2708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4965
_reflns_number_total             6355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00568d2.cif
_cod_data_source_block           a180504b
_cod_depositor_comments
'Adding full bibliography for 7232936--7232938.cif.'
_cod_original_cell_volume        1803.78(17)
_cod_database_code               7232938
_reflns_odcompleteness_completeness 99.97
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C23 = O1-C23A
 1.35 with sigma of 0.01
 O2A-C23A = O2-C23
 1.2 with sigma of 0.01
 C18-C23A = C23-C18
 1.47 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O2A) = Uanis(O2)
Uanis(C23A) = Uanis(C23)
4. Others
 Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
 Sof(O2A)=Sof(C23A)=1-FVAR(2)
 Sof(O2)=Sof(C23)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13C,H13D), C13(H13A,H13B), C24(H24A,H24B), C27(H27A,H27B), C43(H43A,H43B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C15(H15),
 C16(H16), C19(H19), C22(H22), C29(H29), C30(H30), C32(H32), C35(H35), C36(H36),
  C37(H37), C38(H38), C41(H41), C42(H42)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C44(H44A,H44B,H44C), C14(H14A,H14B,
 H14C), C14A(H14D,H14E,H14F)
;
_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 1.364
_oxdiff_exptl_absorpt_empirical_full_min 0.651