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_7223214
_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 Gd2 N4 O12'
_chemical_formula_sum            'C84 H82 Gd2 N4 O12'
_chemical_formula_weight         1654.03
_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                 109.0530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8326(6)
_cell_length_b                   22.9406(10)
_cell_length_c                   13.4767(6)
_cell_measurement_reflns_used    9458
_cell_measurement_temperature    298.84
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.11
_cell_volume                     3750.0(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      298.84
_diffrn_measured_fraction_theta_full 0.998
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49228
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.437
_diffrn_reflns_theta_min         3.089
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_T_max  0.7125
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 6452 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         16962
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0169P)^2^+0.3402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0512
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                14913
_reflns_number_total             16962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14559g2.cif
_cod_data_source_block           7
_cod_database_code               7223214
_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:
 C22(H22), C19(H19), C34(H34), C49(H49), C80(H80), C73(H73)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C20(H20A,H20B), C50(H50A,H50B), C84(H84A,H84B), C74(H74A,
 H74B), C71(H71A,H71B)
2.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C10(H10), C25(H25), C17(H17), C12(H12), C26(H26), C33(H33),
 C32(H32), C16(H16), C11(H11), C37(H37), C38(H38), C54(H54), C53(H53), C52(H52),
  C57(H57), C39(H39), C43(H43), C47(H47), C41(H41), C58(H58), C46(H46),
 C45(H45), C55(H55), C44(H44), C62(H62), C83(H83), C65(H65), C81(H81), C64(H64),
  C63(H63), C79(H79), C77(H77), C75(H75), C61(H61), C68(H68), C60(H60),
 C78(H78), C59(H59), C66(H66), C67(H67), C86(H86), C87(H87), C85(H85), C89(H89),
  C90(H90)
2.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C69(H69A,H69B,H69C), C72(H72A,H72B,H72C), C70(H70A,H70B,
 H70C), C88(H88A,H88B,H88C), C1(H1A,H1B,H1C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'