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_7704794
_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 H86 Dy5 N14 O32, 2(C6 H16 N), H2 O, 2(C2 H3 N), N O3'
_chemical_formula_sum            'C112 H126 Dy5 N19 O36'
_chemical_formula_weight         3126.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   mixed
_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                   28.2054(4)
_cell_length_b                   28.2054(4)
_cell_length_c                   18.1449(3)
_cell_measurement_reflns_used    14866
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.1710
_cell_measurement_theta_min      3.3170
_cell_volume                     14435.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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    -50.00 -23.00   0.50    6.00    --    0.00 -57.00 -90.00   54
  2  \w    -87.00   3.00   0.50    6.00    --    0.00 -57.00-150.00  180
  3  \w    127.00 170.00   0.50   33.00    --   95.80  61.00-180.00   86
  4  \w     68.00  94.00   0.50   33.00    --   95.80  61.00-180.00   52
  5  \w     67.00 184.00   0.50   33.00    --   95.80  45.00 -30.00  234
  6  \w     51.00 125.00   0.50   33.00    --   95.80 -61.00 120.00  148
  7  \w     85.00 160.00   0.50   33.00    --   95.80  45.00   0.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0463139000
_diffrn_orient_matrix_UB_12      -0.0224386000
_diffrn_orient_matrix_UB_13      0.0284621000
_diffrn_orient_matrix_UB_21      -0.0184987000
_diffrn_orient_matrix_UB_22      0.0494945000
_diffrn_orient_matrix_UB_23      0.0214086000
_diffrn_orient_matrix_UB_31      -0.0222955000
_diffrn_orient_matrix_UB_32      0.0053980000
_diffrn_orient_matrix_UB_33      -0.0770640000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49240
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.397
_diffrn_reflns_theta_min         2.896
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    14.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             6196
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.377
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 3060 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         14157
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0587
_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^)+(0.1024P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1661
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                9369
_reflns_number_total             14157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01711f2.cif
_cod_data_source_block           2b_sq
_cod_depositor_comments
'Adding full bibliography for 7704793--7704796.cif.'
_cod_original_cell_volume        14435.1(5)
_cod_database_code               7704794
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.93
_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 C(H,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
 O18-N10 = N10-O19
 1.2 with sigma of 0.02
 N10-O20
 1.2 with sigma of 0.02
 O18-O19
 2.2 with sigma of 0.02
 O20-O19
 2.2 with sigma of 0.02
 O18-O20
 2.2 with sigma of 0.02
 C1-C7 = C7-C1A
 1.4 with sigma of 0.02
 H50C-H19_$1
 2.2 with sigma of 0.02
 O1-H1
 0.85 with sigma of 0.01
 C23-H1
 1.887167 with sigma of 0.02
 Dy2-H1
 3.070849 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim
Ueq, Uanis(C5A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2A) \\sim Ueq,
Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C5, C4, C3, C2, C1, C6, C7, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10, O19, O18, O20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C1, C2, C3, C4, C5A, C4A, C5, C6, C3A, C6A, C2A, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C50, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H7B)=Sof(C1A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=
 Sof(C2A)=Sof(H2A)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(H7A)=Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5A)=Sof(C6)=Sof(H6)=FVAR(1)
 Fixed Sof: O19(0.5) O18(0.5) N10(0.5) O20(0.5)
6.a Riding coordinates:
 O13(H13A,H13B), O5(H5), O14(H14)
6.b Ternary CH refined with riding coordinates:
 N7(H7), C39(H39), C23(H23), C7(H7A), C7(H7B)
6.c Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C49(H49A,H49B), C51(H51A,H51B)
6.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C38(H38), C37(H37), C36(H36), C35(H35), C34(H34), C9(H9), C13(H13),
 C45(H45), C12(H12), C41(H41), C25(H25), C31(H31), C44(H44), C29(H29), C43(H43),
  C30(H30), C19(H19), C20(H20), C21(H21), C22(H22), C18(H18), C2(H2), C3(H3),
 C4(H4), C5(H5A), C6(H6), C3A(H3A), C4A(H4A), C5A(H5AA), C2A(H2A), C6A(H6A)
6.e Fitted hexagon refined as free rotating group:
 C33(C38,C37,C36,C35,C34), C19(C20,C21,C22,C17,C18), C1(C2,C3,C4,C5,C6),
 C1A(C3A,C4A,C5A,C2A,C6A)
6.f Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              854
_shelx_hkl_checksum              93368
_shelx_fab_checksum              75337
_platon_squeeze_void_probe_radius 1.20
_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 2.066
_oxdiff_exptl_absorpt_empirical_full_min 0.430