Homochiral luminescent lanthanide dinuclear complexes derived from a chiral carboxylate
Wen, He-Rui; Xie, Xin-Rong; Liu, Sui-Jun; Bao, Jun; Wang, Feng-Feng; Liu, Cai-Ming; Liao, Jin-Sheng; RSC Adv.  (2015) –; doi:10.1039/C5RA14559G

data_7223215
_publ_section_title
;
 Homochiral luminescent lanthanide dinuclear complexes derived from a
 chiral carboxylate
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA14559G
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C84 H82 N4 O12 Tb2'
_chemical_formula_sum            'C84 H82 N4 O12 Tb2'
_chemical_formula_weight         1657.37
_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             2015-09-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_audit_update_record
;
2015-09-21 deposited with the CCDC.
2015-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.129(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8517(15)
_cell_length_b                   22.976(3)
_cell_length_c                   13.4781(15)
_cell_measurement_reflns_used    9520
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      40.946
_cell_measurement_theta_min      3.104
_cell_volume                     3760.1(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      299.28
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            59972
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.711
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         3.088
_exptl_absorpt_coefficient_mu    1.930
_exptl_absorpt_correction_T_max  0.6988
_exptl_absorpt_correction_T_min  0.6545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.010
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 5809 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.082(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         12565
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+8.8141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                12300
_reflns_number_total             12565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14559g2.cif
_cod_data_source_block           8
_cod_original_cell_volume        3760.1(7)
_cod_database_code               7223215
_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. Rigid bond restraints
 C51, C52, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O10) = Uanis(O11)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C41(H41), C30(H30), C39(H39), C43(H43), C12(H12)
4.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C31(H31A,H31B), C18(H18A,H18B), C45(H45A,H45B), C14(H14A,
 H14B), C58(H58A,H58B)
4.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C10(H10), C28(H28), C8(H8), C19(H19), C3(H3), C27(H27), C21(H21),
 C20(H20), C37(H37), C1(H1), C9(H9), C34(H34), C2(H2), C35(H35), C36(H36),
 C50(H50), C49(H49), C51(H51), C52(H52), C53(H53), C57(H57), C71(H71), C76(H76),
  C75(H75), C65(H65), C69(H69), C48(H48), C77(H77), C72(H72), C54(H54),
 C73(H73), C74(H74), C68(H68), C55(H55), C66(H66), C56(H56), C62(H62), C63(H63),
  C61(H61), C67(H67), C79(H79), C80(H80), C78(H78), C81(H81), C82(H82)
4.d Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C), C84(H84A,H84B,
 H84C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'