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_7223211
_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 Nd2 O12'
_chemical_formula_sum            'C84 H82 N4 Nd2 O12'
_chemical_formula_weight         1628.01
_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                 109.4080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8651(6)
_cell_length_b                   23.1584(10)
_cell_length_c                   13.4478(6)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      27.941
_cell_measurement_theta_min      3.090
_cell_volume                     3778.9(3)
_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      295.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39805
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.089
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.7639
_exptl_absorpt_correction_T_min  0.7264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       block
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.908
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 5311 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         13511
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0330
_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^)+4.8233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                12180
_reflns_number_total             13511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14559g2.cif
_cod_data_source_block           4
_cod_database_code               7223211
_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
 C3-C97 \\sim C97-C3A
 with sigma of 0.02
3. Rigid bond restraints
 C97
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C97, C3A
 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(C90) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H97C)=Sof(H97D)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(H97A)=Sof(H97B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C40(H40), C35(H35), C33(H33), C47(H47), C45(H45), C88(H88)
6.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C49(H49A,H49B), C39(H39A,H39B), C94(H94A,H94B), C89(H89A,
 H89B), C97(H97A,H97B), C97(H97C,H97D)
6.c Aromatic/amide H refined with riding coordinates:
 C56(H56), C52(H52), C21(H21), C23(H23), C51(H51), C29(H29), C31(H31),
 C62(H62), C30(H30), C54(H54), C53(H53), C22(H22), C59(H59), C25(H25), C57(H57),
  C24(H24), C42(H42), C50(H50), C75(H75), C69(H69), C80(H80), C64(H64),
 C92(H92), C77(H77), C66(H66), C68(H68), C73(H73), C72(H72), C81(H81), C63(H63),
  C74(H74), C78(H78), C83(H83), C79(H79), C65(H65), C84(H84), C67(H67),
 C71(H71), C86(H86), C85(H85), C99(H99), C96(H96), C101(H101), C100(H100),
 C102(H102), C95(H95)
6.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C90(H90A,H90B,H90C), C76(H76A,H76B,H76C), C93(H93A,H93B,
 H93C), C82(H82A,H82B,H82C), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'