Dimethylamine substituted bisbenzocoumarins: solvatochromic, mechanochromic and acidochromic properties
Chen, Shaojin; Liu, Wei; Ge, Zhaohai; Zhang, Wenxuan; Wang, Kun-Peng; Hu, Zhi-Qiang; CrystEngComm 20 (2018) 5432–; doi:10.1039/C8CE01034J

data_7231310
_publ_section_title
;
 Dimethylamine substituted bisbenzocoumarins: solvatochromic,
 mechanochromic and acidochromic properties
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5432
_journal_paper_doi               10.1039/C8CE01034J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C36 H32 N2 O8'
_chemical_formula_sum            'C36 H32 N2 O8'
_chemical_formula_weight         620.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-06-18 deposited with the CCDC.
2018-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.466(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.9695(15)
_cell_length_b                   8.1566(5)
_cell_length_c                   12.1516(7)
_cell_measurement_reflns_used    2380
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.0800
_cell_measurement_theta_min      2.9210
_cell_volume                     2970.4(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_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     -7.00  31.00   1.00    6.00    --  -40.98  38.00 120.00   38
  2  \w    -65.00 -32.00   1.00    6.00    --  -40.98  38.00 120.00   33
  3  \w    -94.00  -2.00   1.00    6.00    --  -40.98 125.00 150.00   92
  4  \w   -108.00 -14.00   1.00    6.00    --  -40.98 -57.00 -90.00   94
  5  \w     47.00 109.00   1.00    8.00    --  106.95 -95.00 -30.00   62
  6  \w     43.00 119.00   1.00    8.00    --  106.95-125.00-180.00   76
  7  \w     34.00 129.00   1.00    8.00    --  106.95 -45.00 -60.00   95
  8  \w     81.00 171.00   1.00    8.00    --  106.95  30.00-120.00   90
  9  \w    129.00 156.00   1.00    8.00    --  106.95 125.00   0.00   27
 10  \w     89.00 178.00   1.00    8.00    --  106.95  61.00  90.00   89
;
_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      -0.0258173000
_diffrn_orient_matrix_UB_12      0.1615298000
_diffrn_orient_matrix_UB_13      0.0157139000
_diffrn_orient_matrix_UB_21      0.0380116000
_diffrn_orient_matrix_UB_22      0.0946256000
_diffrn_orient_matrix_UB_23      -0.0562055000
_diffrn_orient_matrix_UB_31      -0.0230465000
_diffrn_orient_matrix_UB_32      -0.0246609000
_diffrn_orient_matrix_UB_33      -0.1126050000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5681
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.381
_diffrn_reflns_theta_min         2.949
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55027
_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    orange
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0743
_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^)+(0.0975P)^2^+20.4213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2377
_reflns_number_total             2896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01034j2.cif
_cod_data_source_block           lw-1
_cod_depositor_comments          'Adding full bibliography for 7231310.cif.'
_cod_original_cell_volume        2970.3(3)
_cod_database_code               7231310
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.895
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C13(H13), C12(H12)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;
_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 2.022
_oxdiff_exptl_absorpt_empirical_full_min 0.164