Ln(III) complexes (Ln = Eu, Gd, Tb, Dy) with chiral ligand containing 1,10-phenanthroline and (–)-menthol fragments: synthesis, structure, magnetic properties and photoluminescence
Larionov, Stanislav V.; Bryleva, Yuliya; Glinskaya, Ludmila Alexsandrovna; Plyusnin, Victor F.; Kupryakov, Arkady S.; Agafontsev, Alexander; Tkachev, Alexey V.; Bogomyakov, Artem Stepanovich; Piryazev, Dmitry A.; Korolkov, Ilya V.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01536D

data_7043902
_publ_section_title
;
 Ln(III) complexes (Ln = Eu, Gd, Tb, Dy) with chiral ligand containing
 1,10-phenanthroline and (--)-menthol fragments: synthesis, structure,
 magnetic properties and photoluminescence
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01536D
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C22 H26 N2 O'
_chemical_formula_sum            'C22 H26 N2 O'
_chemical_formula_weight         334.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-05-26 deposited with the CCDC.
2017-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.270(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.665(2)
_cell_length_b                   15.178(3)
_cell_length_c                   11.980(2)
_cell_measurement_reflns_used    7250
_cell_measurement_temperature    173.0(1)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.17
_cell_volume                     1939.2(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker Apex'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17023
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.431
_diffrn_reflns_theta_min         1.700
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0570 before and 0.0428 after correction. The Ratio of minimum to maximum transmission is 0.8986. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 2800 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.6(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0582P)^2^+1.1242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.910
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                6780
_reflns_number_total             7850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01536d2.cif
_cod_data_source_block           gli451
_cod_original_cell_volume        1939.2(7)
_cod_database_code               7043902
_shelx_shelxl_version_number     2014/7
_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 Ternary CH refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C8(H8), C23(H23), C25(H25), C26(H26), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C24(H24A,H24B), C27(H27A,H27B),
 C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20),
 C34(H34), C35(H35), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'