Radii-dependent self-assembly of chiral lanthanide complexes: synthesis, chirality, and single-molecule magnet behavior.
Li, Ge; Zhao, Xiaoxi; Han, Qingxin; Wang, Li; Liu, Weisheng; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10120–10126; doi:10.1039/d0dt01711f

data_7704795
_publ_section_title
;
 Radii-dependent self-assembly of chiral lanthanide complexes: synthesis,
 chirality, and single-molecule magnet behavior.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10120
_journal_page_last               10126
_journal_paper_doi               10.1039/d0dt01711f
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C96 H88 La3 N12 O24, 7(H2 O), N O3, 4(C2 H3 N)'
_chemical_formula_sum            'C104 H114 La3 N17 O34'
_chemical_formula_weight         2562.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-06-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-25 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6403(11)
_cell_length_b                   26.197(2)
_cell_length_c                   29.383(2)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.486
_cell_measurement_theta_min      2.199
_cell_volume                     11269.3(14)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            62056
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         1.554
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1277 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.7629. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             5200
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 8918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1461
_refine_ls_number_reflns         22165
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0413P)^2^+7.1446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                20739
_reflns_number_total             22165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01711f2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7704793--7704796.cif.'
_cod_original_cell_volume        11269.5(15)
_cod_database_code               7704795
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.859
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O12-H12
 0.85 with sigma of 0.01
 O16-H16
 0.85 with sigma of 0.01
 O29-N13 = N13-O28
 1.2 with sigma of 0.02
 O28-O29 = O29-O30
 2.2 with sigma of 0.02
 N13-O30
 1.2 with sigma of 0.02
 C39-H12
 1.891536 with sigma of 0.02
 La1-H12
 3.253467 with sigma of 0.02
 C55-H16
 1.895934 with sigma of 0.02
 La3-H16
 3.163865 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C97) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C98) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N13) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O30)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N14, C97, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O28, O29, O30, N13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O26(0.5) H26A(0.5) H26B(0.5) O34(0.5) H34A(0.5) H34B(0.5) O35(0.5)
 H35A(0.5) H35B(0.5) O36(0.5) H36A(0.5) H36B(0.5)
6.a Riding coordinates:
 O25(H25A,H25B), O26(H26A,H26B), O27(H27A,H27B), O31(H31A,H31B), O32(H32D,
 H32E), O33(H33A,H33B), O34(H34A,H34B), O35(H35A,H35B), O36(H36A,H36B)
6.b Ternary CH refined with riding coordinates:
 C9(H9), C24(H24A), C39(H39), C55(H55), C71(H71), C87(H87)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4A), N10(H10), N12(H12A), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8A),
  C11(H11), C15(H15), C16(H16A), C17(H17), C19(H19), C20(H20A), C21(H21),
 C22(H22), C23(H23), C26(H26), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C41(H41), C43(H43), C44(H44), C45(H45),
 C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C57(H57), C59(H59), C60(H60),
  C61(H61), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C73(H73),
 C77(H77), C78(H78), C79(H79), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
  C89(H89), C91(H91), C92(H92), C93(H93)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C32(H32A,H32B,H32C), C48(H48A,H48B,H48C), C64(H64A,H64B,
 H64C), C80(H80A,H80B,H80C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C),
 C100(H10A,H10B,H10C), C102(H10D,H10E,H10F), C104(H10G,H10H,H10I)
6.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O8(H8), O20(H20), O24(H24)
;
_shelx_res_checksum              75295
_shelx_hkl_checksum              12626
_olex2_submission_special_instructions 'No special instructions were received'