Spiro[pyrrol-benzopyran] Based Probe with High Asymmetry for Chiroptical Sensing via Circular Dichroism
Tan, Jingyun; Wang, Chunfei; Lao, Hio Kuan; Wang, Wenjing; Feng, Gang; Yuan, Daqiang; Wu, Changfeng; Zhang, Xuanjun; Chemical Communications  (2019) –; doi:10.1039/C9CC02946J

data_7123515
_publ_section_title
;
 Spiro[pyrrol-benzopyran] Based Probe with High Asymmetry for Chiroptical
 Sensing via Circular Dichroism
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02946J
_journal_year                    2019
_chemical_formula_moiety         'C29 H21 N5 O2 S, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C29.5 H22 Cl N5 O2 S'
_chemical_formula_weight         546.03
_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_method           SHELXL-2017/1
_audit_update_record
;
2019-04-08 deposited with the CCDC.    2019-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                82.255(3)
_cell_angle_beta                 80.785(2)
_cell_angle_gamma                79.244(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0089(2)
_cell_length_b                   12.1459(4)
_cell_length_c                   13.9061(4)
_cell_measurement_reflns_used    12115
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.4760
_cell_measurement_theta_min      4.6460
_cell_volume                     1304.11(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21033
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.779
_diffrn_reflns_theta_min         3.726
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81137
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       prism
_exptl_crystal_F_000             566
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, toluene'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.319
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0577
_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^)+(0.1020P)^2^+1.9283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4916
_reflns_number_total             5161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02946j2.cif
_cod_data_source_block           EPMO2
_cod_original_formula_sum        'C29.50 H22 Cl N5 O2 S'
_cod_database_code               7123515
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              79989