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_7223212
_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 Sm2'
_chemical_formula_sum            'C84 H82 N4 O12 Sm2'
_chemical_formula_weight         1640.23
_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                 109.337(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.810(2)
_cell_length_b                   23.160(4)
_cell_length_c                   13.434(2)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    299.26
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      3.09
_cell_volume                     3760.8(10)
_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      299.26
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0458
_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       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43590
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.089
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_T_max  0.7389
_exptl_absorpt_correction_T_min  0.6985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 5133 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         14257
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0244P)^2^+0.0630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.942
_reflns_friedel_fraction_full    0.992
_reflns_friedel_fraction_max     0.992
_reflns_number_gt                12209
_reflns_number_total             14257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14559g2.cif
_cod_data_source_block           5
_cod_original_cell_volume        3761.0(10)
_cod_database_code               7223212
_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-C155 \\sim C155-C3A
 with sigma of 0.02
 C0AA-C148 \\sim C148-C0AB
 with sigma of 0.02
3. Rigid bond restraints
 C3, C155, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C148, C0AA, C0AB
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C172, C175
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(H15C)=Sof(H15D)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
 Sof(H14C)=Sof(H14D)=Sof(C0AB)=Sof(H0AD)=Sof(H0AE)=Sof(H0AF)=1-FVAR(2)
 Sof(H14A)=Sof(H14B)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C81(H81), C97(H97), C88(H88), C114(H114), C118(H118), C152(H152)
5.b Secondary CH2 refined with riding coordinates:
 C98(H98A,H98B), C89(H89A,H89B), C133(H13A,H13B), C155(H15A,H15B), C155(H15C,
 H15D), C148(H14C,H14D), C148(H14A,H14B), C168(H16D,H16E)
5.c Aromatic/amide H refined with riding coordinates:
 C113(H113), C132(H132), C129(H129), C111(H111), C105(H105), C125(H125),
 C106(H106), C107(H107), C131(H131), C124(H124), C112(H112), C110(H110),
 C122(H122), C109(H109), C130(H130), C128(H128), C120(H120), C126(H126),
 C117(H117), C121(H121), C136(H136), C137(H137), C116(H116), C135(H135),
 C123(H123), C157(H157), C156(H156), C139(H139), C141(H141), C143(H143),
 C140(H140), C147(H147), C144(H144), C146(H146), C145(H145), C159(H159),
 C162(H162), C163(H163), C160(H160), C158(H158), C166(H166), C172(H172),
 C171(H171), C173(H173), C174(H174), C175(H175)
5.d Idealised Me refined as rotating group:
 C99(H99A,H99B,H99C), C161(H16A,H16B,H16C), C169(H16F,H16G,H16H), C167(H16I,
 H16J,H16K), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C0AA(H0AA,H0AB,H0AC),
 C0AB(H0AD,H0AE,H0AF)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'