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_7701198
_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_absolute_configuration ad
_chemical_formula_moiety
'C120 H104 Dy4 N16 O25, 2(N O3), 5(H2 O), C2 H3 N'
_chemical_formula_sum            'C122 H117 Dy4 N19 O36'
_chemical_formula_weight         3075.34
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-08-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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            4
_cell_length_a                   16.5304(4)
_cell_length_b                   21.5083(5)
_cell_length_c                   34.7813(7)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      66.626
_cell_measurement_theta_min      2.960
_cell_volume                     12366.2(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            92156
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        66.632
_diffrn_reflns_theta_max         66.632
_diffrn_reflns_theta_min         2.415
_exptl_absorpt_coefficient_mu    13.459
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1465 before and 0.0998 after correction.
The Ratio of minimum to maximum transmission is 0.5264.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             6136
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.685
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.050(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1918
_refine_ls_number_reflns         20869
_refine_ls_number_restraints     1794
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+28.6735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.903
_reflns_number_gt                19872
_reflns_number_total             20869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02483b2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7701197--7701200.cif.'
_cod_database_code               7701198
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.274
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.950(4)
 0.050(4)
2. 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
3. Restrained distances
 O36-N19 = N19-O35
 1.2 with sigma of 0.02
 N19-O34
 1.2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N23) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(O25)
\\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq,
Uanis(C70) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N19) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O36)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C52A) \\sim Ueq,
Uanis(C57A) \\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(C55A) \\sim Ueq,
Uanis(C54A) \\sim Ueq, Uanis(C53A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C68A) \\sim Ueq,
Uanis(C69A) \\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C71A) \\sim Ueq,
Uanis(C72A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C82A)
\\sim Ueq, Uanis(C86A) \\sim Ueq, Uanis(C87A) \\sim Ueq, Uanis(C83) \\sim Ueq,
Uanis(C83A) \\sim Ueq, Uanis(C84A) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C85A) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C1A) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C1B)
\\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C1D) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C1E) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(O39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49,
 C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64, C65,
  C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79, C80,
 C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92, C93, C94, C95, C96,
  C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, C107, C108, C109,
 C110, C111, C112, C113, C114, C115, C116, C117, C118, C119, C120, C121, C122,
 C124, C125, C126, C82A, C83A, C84A, C85A, C86A, C87A, C52A, C57A, C56A, C55A,
 C54A, C53A, C51A, C68A, C69A, C70A, C71A, C72A, C1A, C1B, C1C, C1D, C1E, N1,
 N2, N3, N4, N5, N7, N8, N9, N10, N11, N12, N13, N14, N15, N16, N20, N17, N18,
 N21, N19, N23, O1, O2, O3, O4, O5, O6, O7, O8, O9, O10, O11, O12, O13, O14,
 O15, O16, O17, O18, O19, O20, O21, O22, O23, O24, O37, O25, O26, O27, O28, O29,
  O30, O31, O32, O33, O35, O34, O36, O38, O39, O14A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(H81A)=Sof(C82A)=Sof(C83A)=Sof(H83A)=Sof(C84A)=Sof(H84A)=Sof(C85A)=
 Sof(H85A)=Sof(C86A)=Sof(H86A)=Sof(C87A)=Sof(H87A)=1-FVAR(1)
 Sof(H81)=Sof(C82)=Sof(C83)=Sof(H83)=Sof(C84)=Sof(H84)=Sof(C85)=Sof(H85)=
 Sof(C86)=Sof(H86)=Sof(C87)=Sof(H87)=FVAR(1)
 Sof(C52A)=Sof(C57A)=Sof(H57A)=Sof(C56A)=Sof(H56A)=Sof(C55A)=Sof(H55A)=
 Sof(C54A)=Sof(H54A)=Sof(C53A)=Sof(H53A)=Sof(C51A)=Sof(H51A)=Sof(O14A)=
 Sof(H14B)=1-FVAR(2)
 Sof(O14)=Sof(H14)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(C53)=Sof(H53)=Sof(C54)=
 Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=FVAR(2)
 Sof(C68A)=Sof(H68A)=Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(H70A)=Sof(C71A)=
 Sof(H71A)=Sof(C72A)=Sof(H72A)=1-FVAR(3)
 Sof(C68)=Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71)=
 Sof(C72)=Sof(H72)=FVAR(3)
 Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(H1B)=Sof(C1C)=Sof(H1C)=Sof(C1D)=Sof(H1D)=
 Sof(C1E)=Sof(H1E)=1-FVAR(4)
 Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=Sof(C104)=Sof(H104)=Sof(C105)=
 Sof(H105)=Sof(C106)=Sof(H106)=FVAR(4)
 Fixed Sof: O25(0.5) O26(0.5) O27(0.5) N17(0.5) C122(0.5) N21(0.5) C124(0.5)
 H12B(0.5) H12C(0.5) H12D(0.5) O35(0.5) N19(0.5) O34(0.5) O36(0.5) C125(0.5)
 N23(0.5) C126(0.5) H12E(0.5) H12F(0.5) H12G(0.5)
7.a Riding coordinates:
 O4(H4), O7(H7), O10(H10), O17(H17), O20(H20), O22(H22), O24(H24), O31(H31A,
 H31B), O32(H32A,H32B), O33(H33A,H33B), O38(H38A,H38B), O39(H39A,H39B)
7.b Ternary CH refined with riding coordinates:
 C5(H5A), C20(H20A), C36(H36), C51(H51), C66(H66), C81(H81), C81(H81A),
 C100(H100), C115(H115), C51A(H51A)
7.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4A), N5(H5), N8(H8), N10(H10A), N12(H12), N13(H13), N15(H15),
 C3(H3), C7(H7A), C8(H8A), C9(H9), C10(H10B), C11(H11), C12(H12A), C13(H13A),
 C14(H14A), C15(H15A), C18(H18), C22(H22A), C23(H23), C24(H24A), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C49(H49), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
  C60(H60), C61(H61), C64(H64), C68(H68), C69(H69), C70(H70), C71(H71),
 C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C79(H79), C83(H83), C84(H84),
  C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91),
 C93(H93), C96(H96), C97(H97), C98(H98), C99(H99), C102(H102), C103(H103),
 C104(H104), C105(H105), C106(H106), C108(H108), C111(H111), C112(H112),
 C113(H113), C114(H114), C117(H117), C118(H118), C119(H119), C120(H120),
 C121(H121), C83A(H83A), C84A(H84A), C85A(H85A), C86A(H86A), C87A(H87A),
 C57A(H57A), C56A(H56A), C55A(H55A), C54A(H54A), C53A(H53A), C68A(H68A),
 C69A(H69A), C70A(H70A), C71A(H71A), C72A(H72A), C1A(H1A), C1B(H1B), C1C(H1C),
 C1D(H1D), C1E(H1E)
7.d Idealised Me refined as rotating group:
 C124(H12B,H12C,H12D), C126(H12E,H12F,H12G)
7.e Idealised tetrahedral OH refined as rotating group:
 O14(H14), O14A(H14B)
;
_shelx_res_checksum              79927
_olex2_submission_special_instructions 'No special instructions were received'