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_7223213
_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 Eu2 N4 O12'
_chemical_formula_sum            'C84 H82 Eu2 N4 O12'
_chemical_formula_weight         1643.45
_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             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                 109.241(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7972(17)
_cell_length_b                   23.189(3)
_cell_length_c                   13.4405(18)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.82
_cell_volume                     3765.7(9)
_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      298.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            55881
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.256
_diffrn_reflns_theta_max         24.256
_diffrn_reflns_theta_min         3.086
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_T_max  0.7255
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_refine_diff_density_max         2.593
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 5258 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         11998
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+11.7581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                11356
_reflns_number_total             11998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14559g2.cif
_cod_data_source_block           6
_cod_original_cell_volume        3765.8(9)
_cod_database_code               7223213
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C62-C114
 1.4 with sigma of 0.01
 C62-C114
 1.41 with sigma of 0.02
 C4A-C126 \\sim C126-C4
 with sigma of 0.02
3. Rigid bond restraints
 C84, C85
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C115, C116, C117, C118
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C127
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H12H)=Sof(H12I)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(H12F)=Sof(H12G)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C43(H43), C52(H52), C61(H61), C66(H66), C96(H96), C83(H83)
6.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C45(H45A,H45B), C78(H78A,H78B), C100(H10A,H10B), C127(H12A,
 H12B), C126(H12F,H12G), C126(H12H,H12I)
6.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C68(H68), C106(H106), C107(H107), C104(H104), C105(H105), C49(H49),
 C48(H48), C50(H50), C51(H51), C57(H57), C46(H46), C69(H69), C77(H77), C75(H75),
  C70(H70), C86(H86), C76(H76), C72(H72), C73(H73), C85(H85), C115(H115),
 C117(H117), C116(H116), C118(H118), C92(H92), C88(H88), C87(H87), C99(H99),
 C91(H91), C98(H98), C90(H90), C109(H109), C120(H120), C110(H110), C119(H119),
 C121(H121), C122(H122), C125(H125), C108(H108), C114(H114), C124(H124),
 C111(H111), C113(H113), C131(H131), C130(H130)
6.d Fitted hexagon refined as free rotating group:
 C68(C106,C103,C107,C104,C105), C85(C84,C115,C117,C116,C118)
6.e Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C123(H12C,H12D,H12E), C129(H12J,H12K,H12L), C128(H12M,
 H12N,H12O), C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC), C3(H3A,H3B,H3C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'