Construction of homochiral alkaline-lanthanide heteronuclear helicates with Na<sup>+</sup>-selective bonding in the self-assembly process.
Li, Ge; Wang, Li; Han, Qingxin; Liu, Weisheng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14595–14599; doi:10.1039/c9dt02483b

data_7701197
_publ_section_title
;
 Construction of homochiral alkaline-lanthanide heteronuclear helicates
 with Na<sup>+</sup>-selective bonding in the self-assembly process.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14595
_journal_page_last               14599
_journal_paper_doi               10.1039/c9dt02483b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'2(C48 H45 Dy N6 Na1.5 O12), H N0.5 O2, 2(N O3)'
_chemical_formula_sum            'C96 H91 Dy2 N14.5 Na3 O32'
_chemical_formula_weight         2353.80
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-15
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.31 svn.r3643 for OlexSys, GUI svn.r5859)
;
_audit_update_record
;
2019-08-20 deposited with the CCDC.    2019-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.876(6)
_cell_length_b                   20.204(5)
_cell_length_c                   56.153(14)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.191
_cell_measurement_theta_min      2.272
_cell_volume                     24819(11)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            61577
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         0.725
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.6694.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             9516
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.076
_refine_diff_density_min         -2.670
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.070(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1335
_refine_ls_number_reflns         21795
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0481P)^2^+226.9290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                20209
_reflns_number_total             21795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02483b2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7701197--7701200.cif.'
_cod_original_formula_sum        'C96 H91 Dy2 N14.50 Na3 O32'
_cod_database_code               7701197
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.930(13)
 0.070(13)
2. 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
3. Restrained distances
 H6-O26
 2 with sigma of 0.02
 N13-O25
 1.2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C62) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C65) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O6) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C62, C60, C59, C61, C63, C64
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C32, C31, C30, C28, C29, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N13, O25, O26, O27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H25A(0.5) H25B(0.5) O26(0.5) O27(0.5) N13(0.5)
7.a Riding coordinates:
 O12(H12), O21(H21A), O24(H24A), O18(H18), O25(H25A,H25B)
7.b Ternary CH refined with riding coordinates:
 C26(H26), C10(H10), C42(H42), C86(H86), C58(H58), C70(H70)
7.c Aromatic/amide H refined with riding coordinates:
 N6(H6A), N4(H4), N2(H2), C40(H40), C24(H24), C8(H8), C37(H37), C46(H46),
 C20(H20), C21(H21), C28(H28), C36(H36), C38(H38), C47(H47), C48(H48), C31(H31),
  C15(H15), C32(H32), C12(H12A), C29(H29), C14(H14), C30(H30), C13(H13),
 C16(H16), C6(H6B), C5(H5), C4(H4A), C22(H22), C45(H45), C44(H44), N12(H12B),
 N10(H10A), N8(H8A), C62(H62), C61(H61), C60(H60), C64(H64), C63(H63), C74(H74),
  C56(H56), C54(H54), C88(H88), C68(H68), C93(H93), C53(H53), C84(H84),
 C77(H77), C92(H92), C72(H72), C78(H78), C90(H90), C89(H89), C52(H52), C79(H79),
  C95(H95), C91(H91), C73(H73), C75(H75), C76(H76), C94(H94)
7.d Fitted hexagon refined as free rotating group:
 C62(C61,C60,C59,C64,C63)
7.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C3(H3A,H3B,H3C), C35(H35A,H35B,H35C), C96(H96A,H96B,
 H96C), C51(H51A,H51B,H51C), C80(H80A,H80B,H80C)
7.f Idealised tetrahedral OH refined as rotating group:
 O9(H9), O6(H6)
;
_shelx_res_checksum              62830
_shelx_fab_checksum              63558
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'