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_7704796
_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, 8(H2 O), N O2, 4(C2 H3 N)'
_chemical_formula_sum            'C104 H116 La3 N17 O34'
_chemical_formula_weight         2564.86
_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     dual
_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                   14.66180(10)
_cell_length_b                   26.22330(10)
_cell_length_c                   29.37640(10)
_cell_measurement_reflns_used    94814
_cell_measurement_temperature    293
_cell_measurement_theta_max      74.1890
_cell_measurement_theta_min      2.948
_cell_volume                     11294.66(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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    'ShelXS 2018/3 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     52.00  88.00   0.50    0.50    --    0.00  82.00-180.00   72
  2  \w     13.00  39.00   0.50    0.50    --    0.00  82.00-180.00   52
  3  \w    -16.00  43.00   0.50    0.50    --    0.00  38.00 120.00  118
  4  \w    -88.00 -62.00   0.50    0.50    --    0.00 -38.00-180.00   52
  5  \w     82.00 153.00   0.50    1.44    --   95.20  30.00  90.00  142
  6  \w      6.00 126.00   0.50    1.44    --   95.20 -82.00  30.00  240
  7  \w    100.00 185.00   0.50    1.44    --   95.20  30.00 120.00  170
  8  \w     52.00 109.00   0.50    1.44    --   95.20 -61.00  30.00  114
  9  \w    -63.00 -32.00   0.50    0.50    --    0.00 -57.00  30.00   62
 10  \w    -41.00  20.00   0.50    0.50    --    0.00 -82.00 -30.00  122
 11  \w    -48.00 -22.00   0.50    0.50    --    0.00 -38.00-120.00   52
 12  \w    -88.00 -26.00   0.50    0.50    --    0.00 -38.00-150.00  124
 13  \w    -30.00  20.00   0.50    0.50    --    0.00 -57.00  30.00  100
 14  \w     83.00 181.00   0.50    1.44    --   95.20  30.00 -30.00  196
 15  \w      7.00 120.00   0.50    1.44    --   95.20 -82.00 -90.00  226
 16  \w     17.00 108.00   0.50    1.44    --   95.20 -82.00-180.00  182
 17  \w    143.00 182.00   0.50    1.44    --   95.20  77.00-180.00   78
 18  \w     67.00 102.00   0.50    1.44    --   95.20  77.00-180.00   70
 19  \w     16.00  55.00   0.50    1.44    --   95.20 -45.00 120.00   78
 20  \w     89.00 114.00   0.50    1.44    --   95.20 -45.00 120.00   50
 21  \w     92.00 119.00   0.50    1.44    --   95.20 -15.00   0.00   54
 22  \w     16.00 102.00   0.50    1.44    --   95.20 -61.00 -90.00  172
 23  \w     95.00 124.00   0.50    1.44    --   95.20  61.00-180.00   58
 24  \w     25.00  70.00   0.50    1.44    --   95.20 -82.00 150.00   90
 25  \w    122.00 184.00   0.50    1.44    --   95.20  30.00  30.00  124
 26  \w     45.00  88.00   0.50    1.44    --   95.20 -15.00   0.00   86
 27  \w     11.00  37.00   0.50    1.44    --   95.20 -77.00  90.00   52
 28  \w     74.00 100.00   0.50    1.44    --   95.20 -77.00  90.00   52
 29  \w     80.00 183.00   0.50    1.44    --   95.20  30.00   0.00  206
 30  \w     34.00 111.00   0.50    1.44    --   95.20 -61.00-180.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0949074000
_diffrn_orient_matrix_UB_12      0.0038743000
_diffrn_orient_matrix_UB_13      -0.0222586000
_diffrn_orient_matrix_UB_21      -0.0160394000
_diffrn_orient_matrix_UB_22      -0.0571384000
_diffrn_orient_matrix_UB_23      0.0091603000
_diffrn_orient_matrix_UB_31      -0.0422225000
_diffrn_orient_matrix_UB_32      0.0130777000
_diffrn_orient_matrix_UB_33      0.0465723000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            142478
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.113
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.335
_exptl_absorpt_correction_T_max  0.33280
_exptl_absorpt_correction_T_min  0.27431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             5208
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.290
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 9468 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0055(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1470
_refine_ls_number_reflns         22207
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0656P)^2^+19.5300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                21683
_reflns_number_total             22207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01711f2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7704793--7704796.cif.'
_cod_database_code               7704796
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.455
_shelx_estimated_absorpt_t_min   0.377
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 C(H,H,H,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
 C97A-N14A
 1.2 with sigma of 0.02
 C97A-C98
 1.5 with sigma of 0.02
 O28-N13 = N13-O29
 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, Uanis(N13)
\\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O36) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O31) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O32)
\\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
 N16, C101, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O28, O29, N13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H98D)=Sof(H98E)=Sof(H98F)=Sof(C97A)=Sof(N14A)=1-FVAR(1)
 Sof(N14)=Sof(C97)=Sof(H98A)=Sof(H98B)=Sof(H98C)=FVAR(1)
 Fixed Sof: O31(0.75) H31A(0.75) H31B(0.75) O34(0.75) H34A(0.75) H34B(0.75)
 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),
 C98(H98A,H98B,H98C), C98(H98D,H98E,H98F)
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), 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              34327
_shelx_hkl_checksum              99750
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.687
_oxdiff_exptl_absorpt_empirical_full_min 0.507