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_7223210
_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 Pr2'
_chemical_formula_sum            'C84 H82 N4 O12 Pr2'
_chemical_formula_weight         1621.35
_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                 109.2870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8915(6)
_cell_length_b                   23.1403(11)
_cell_length_c                   13.4533(6)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    297.65
_cell_measurement_theta_max      24.578
_cell_measurement_theta_min      3.090
_cell_volume                     3788.1(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      297.65
_diffrn_measured_fraction_theta_full 0.996
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            54462
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.685
_diffrn_reflns_theta_max         24.685
_diffrn_reflns_theta_min         2.674
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_T_max  0.9738
_exptl_absorpt_correction_T_min  0.7400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 4247 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         12790
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.942
_reflns_friedel_fraction_full    0.992
_reflns_friedel_fraction_max     0.992
_reflns_number_gt                10364
_reflns_number_total             12790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14559g2.cif
_cod_data_source_block           3
_cod_database_code               7223210
_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
 C92-C31
 1.4 with sigma of 0.001
 C3-C103 \\sim C103-C3A
 with sigma of 0.02
3. Rigid bond restraints
 C98, C99, C100, C96, C97
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C103, 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(C97) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(H10C)=Sof(H10D)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(H10A)=Sof(H10B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C25(H25), C45(H45), C53(H53), C58(H58), C66(H66)
6.b Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C62(H62A,H62B), C78(H78A,H78B), C90(H90A,H90B), C103(H10A,
 H10B), C103(H10C,H10D), C96(H96A,H96B)
6.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C32(H32), C36(H36), C33(H33), C37(H37), C43(H43), C51(H51),
 C46(H46), C42(H42), C49(H49), C41(H41), C50(H50), C47(H47), C52(H52), C57(H57),
  C56(H56), C55(H55), C65(H65), C68(H68), C64(H64), C63(H63), C60(H60),
 C61(H61), C81(H81), C75(H75), C73(H73), C74(H74), C80(H80), C82(H82), C77(H77),
  C76(H76), C84(H84), C85(H85), C102(H102), C88(H88), C87(H87), C100(H100),
 C83(H83), C98(H98), C92(H92), C93(H93), C99(H99), C95(H95), C101(H101),
 C86(H86), C94(H94)
6.d Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C79(H79A,H79B,H79C), C89(H89A,H89B,H89C), C91(H91A,H91B,
 H91C), C97(H97A,H97B,H97C), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'