Novel asymmetric photodimerization reaction of coumarin derivatives bearing a chiral 2-oxazolidinone auxiliary
Itoh, Kennosuke; Odate, Fumiya; Karikomi, Takuma; Obe, Keishi; Miyamori, Tsutomu; Kamiya, Hideaki; Yoza, Kenji; Nagai, Kenichiro; Fujii, Hideaki; Suga, Hiroyuki; Tokunaga, Ken; RSC Advances 9 (2019) 12365–; doi:10.1039/C9RA00822E

data_7232652
_publ_section_title
;
 Novel asymmetric photodimerization reaction of coumarin derivatives
 bearing a chiral 2-oxazolidinone auxiliary
;
_journal_issue                   22
_journal_name_full               'RSC Advances'
_journal_page_first              12365
_journal_paper_doi               10.1039/C9RA00822E
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C40 H29 Cl3 N2 O10'
_chemical_formula_weight         804.00
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-05-26 deposited with the CCDC.    2019-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.620(5)
_cell_length_b                   15.369(6)
_cell_length_c                   21.972(9)
_cell_measurement_temperature    296(2)
_cell_volume                     3586(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_unetI/netI     0.1303
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17425
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.080
_diffrn_reflns_theta_min         1.617
_exptl_absorpt_coefficient_mu    0.321
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             1656
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Flack x determined using 1261 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.02(8)
_refine_ls_extinction_coef       0.020(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         6314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1490
_refine_ls_R_factor_gt           0.0956
_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^)+(0.1674P)^2^+5.3780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2672
_refine_ls_wR_factor_ref         0.3010
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                3951
_reflns_number_total             6314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra00822e2.cif
_cod_data_source_block           p212121_a
_cod_database_code               7232652
_shelxl_version_number           2013-4
_shelx_res_checksum              56640