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_7223217
_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 Ho2 N4 O12'
_chemical_formula_sum            'C84 H82 Ho2 N4 O12'
_chemical_formula_weight         1669.39
_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             2015-09-21
_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                 109.174(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.819(3)
_cell_length_b                   22.916(4)
_cell_length_c                   13.425(3)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      27.260
_cell_measurement_theta_min      3.114
_cell_volume                     3725.0(14)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      301.0
_diffrn_measured_fraction_theta_full 0.997
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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            48849
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         3.099
_exptl_absorpt_coefficient_mu    2.174
_exptl_absorpt_correction_T_max  0.6957
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 4625 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         16991
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0136P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                12355
_reflns_number_total             16991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14559g2.cif
_cod_data_source_block           10
_cod_original_cell_volume        3725.0(12)
_cod_database_code               7223217
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.646
_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:
 C14(H14), C64(H64), C34(H34), C44(H44), C54(H54), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C71(H71A,H71B), C61(H61A,H61B), C51(H51A,H51B), C31(H31A,
 H31B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C80(H80), C82(H82), C81(H81), C3(H3), C1(H1), C73(H73), C5(H5), C6(H6),
 C75(H75), C78(H78), C77(H77), C36(H36), C74(H74), C20(H20), C70(H70), C66(H66),
  C16(H16), C46(H46), C56(H56), C37(H37), C40(H40), C67(H67), C50(H50),
 C58(H58), C10(H10), C19(H19), C60(H60), C38(H38), C59(H59), C57(H57), C39(H39),
  C68(H68), C8(H8), C9(H9), C18(H18), C47(H47), C69(H69), C17(H17), C2(H2),
 C49(H49), C30(H30), C48(H48), C29(H29), C27(H27), C26(H26), C28(H28)
2.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C72(H72A,H72B,H72C), C52(H52A,H52B,H52C), C42(H42A,H42B,
 H42C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'