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_7223209
_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 Ce2 N4 O12'
_chemical_formula_sum            'C84 H82 Ce2 N4 O12'
_chemical_formula_weight         1619.77
_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                 109.1570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9263(7)
_cell_length_b                   23.1494(14)
_cell_length_c                   13.4675(8)
_cell_measurement_reflns_used    9084
_cell_measurement_temperature    297.7
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      3.09
_cell_volume                     3806.8(4)
_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      297.7
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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            53629
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.407
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         3.088
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.7889
_exptl_absorpt_correction_T_min  0.7544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 5086 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   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         12468
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0145P)^2^+2.9585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                11277
_reflns_number_total             12468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14559g2.cif
_cod_data_source_block           2
_cod_database_code               7223209
_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
 C0AA-C81 \\sim C81-C0AB
 with sigma of 0.02
 C8-C94 \\sim C94-C8A
 with sigma of 0.02
3. Rigid bond restraints
 C0AA, C81, C0AB
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C94, C8A, C82, C90
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(H81C)=Sof(H81D)=Sof(C0AB)=Sof(H0AD)=Sof(H0AE)=Sof(H0AF)=1-FVAR(1)
 Sof(H81A)=Sof(H81B)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=FVAR(1)
 Sof(H94C)=Sof(H94D)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(2)
 Sof(H94A)=Sof(H94B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C27(H27), C26(H26), C32(H32), C66(H66), C80(H80)
5.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C55(H55A,H55B), C71(H71A,H71B), C67(H67A,H67B), C81(H81A,
 H81B), C81(H81C,H81D), C94(H94A,H94B), C94(H94C,H94D)
5.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C35(H35), C34(H34), C65(H65), C64(H64), C63(H63), C39(H39),
 C42(H42), C59(H59), C53(H53), C61(H61), C47(H47), C43(H43), C54(H54), C58(H58),
  C70(H70), C50(H50), C60(H60), C45(H45), C40(H40), C51(H51), C46(H46),
 C52(H52), C69(H69), C56(H56), C49(H49), C87(H87), C83(H83), C84(H84), C85(H85),
  C86(H86), C75(H75), C73(H73), C82(H82), C74(H74), C78(H78), C88(H88),
 C95(H95), C97(H97), C91(H91), C96(H96), C90(H90), C92(H92), C101(H101),
 C98(H98), C100(H100)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C89(H89A,H89B,H89C), C72(H72A,H72B,H72C), C93(H93A,H93B,
 H93C), C0AA(H0AA,H0AB,H0AC), C0AB(H0AD,H0AE,H0AF), C8(H8A,H8B,H8C), C8A(H8AA,
 H8AB,H8AC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'