Lanthanide complexes combined with chiral salen ligands: application in the enantioselective epoxidation reaction of α,β-unsaturated ketones
Xia, Xuexiu; Lu, Chengrong; Zhao, Bei; Yao, Yingming; RSC Advances 9 (2019) 13749–; doi:10.1039/C9RA01529A

data_7232719
_publ_section_title
;
 Lanthanide complexes combined with chiral salen ligands: application in
 the enantioselective epoxidation reaction of \a,\b-unsaturated ketones
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              13749
_journal_paper_doi               10.1039/C9RA01529A
_journal_volume                  9
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_sum            'C16 H14 O3'
_chemical_formula_weight         254.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-01-05 deposited with the CCDC.    2019-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.639(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.6601(8)
_cell_length_b                   5.7080(2)
_cell_length_c                   15.2031(4)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      3.43
_cell_volume                     2535.75(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21056
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         3.025
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.6483
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1815 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4614
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0728P)^2^+1.9830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4333
_reflns_number_total             4614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra01529a2.cif
_cod_data_source_block           1215-2
_cod_database_code               7232719
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              84353