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_7701200
_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, C H4 O, 3(N O3), 4(H2 O)'
_chemical_formula_sum            'C121 H116 Dy4 N19 O39'
_chemical_formula_weight         3110.32
_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
_audit_creation_date             2019-08-13
_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                   16.4632(2)
_cell_length_b                   21.6760(4)
_cell_length_c                   34.7600(6)
_cell_measurement_reflns_used    23362
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2920
_cell_measurement_theta_min      1.9700
_cell_volume                     12404.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5368
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -14.00  84.10   0.30    2.50    --   11.74  57.00  60.00  327
  2  \w     35.00  60.80   0.30    2.50    --   11.74 178.00-120.00   86
  3  \w    -15.00  79.20   0.30    2.50    --   11.74  77.00-180.00  314
  4  \w    -55.00   5.30   0.30    2.50    --   11.74 -57.00 -90.00  201
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0282510000
_diffrn_orient_matrix_UB_12      -0.0064139000
_diffrn_orient_matrix_UB_13      0.0148813000
_diffrn_orient_matrix_UB_21      -0.0304200000
_diffrn_orient_matrix_UB_22      0.0059687000
_diffrn_orient_matrix_UB_23      0.0139576000
_diffrn_orient_matrix_UB_31      -0.0115014000
_diffrn_orient_matrix_UB_32      -0.0315318000
_diffrn_orient_matrix_UB_33      -0.0003820000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0619
_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       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            79531
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.946
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.665
_exptl_crystal_description       block
_exptl_crystal_F_000             6204
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.484
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 6980 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1662
_refine_ls_number_reflns         21873
_refine_ls_number_restraints     1164
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0611P)^2^+62.7325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                18330
_reflns_number_total             21873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02483b2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7701197--7701200.cif.'
_cod_original_cell_volume        12404.3(4)
_cod_database_code               7701200
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.739
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C11-C12
 1.4 with sigma of 0.02
 C12-C13
 1.4 with sigma of 0.02
 C13-C14
 1.4 with sigma of 0.02
 C14-C13
 1.4 with sigma of 0.02
 C13-C12
 1.4 with sigma of 0.02
 C12-C11
 1.4 with sigma of 0.02
 O35-N19 \\sim N19-O36
 with sigma of 0.02
 O37-N19 \\sim N19-O36
 with sigma of 0.02
 O32-N18 \\sim N18-O33
 with sigma of 0.02
 O34-N18 \\sim N18-O33
 with sigma of 0.02
 O37-O35 \\sim O35-O36
 with sigma of 0.02
 O35-O37 \\sim O37-O36
 with sigma of 0.02
 O34-O33 \\sim O33-O32
 with sigma of 0.02
 O34-O32 \\sim O32-O33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01
Uanis(N12A) \\sim Ueq, Uanis(N12) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(N6) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O39) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(N19) \\sim Ueq, Uanis(O37)
\\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O38) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: N12(0.5) H12(0.5) N12A(0.5) H12A(0.5)
5.a Riding coordinates:
 O4(H4), O10(H10), O13(H13), O19(H19), O22(H22), O30(H30A,H30B), O31(H31A,
 H31B), O38(H38A,H38B), O39(H39A,H39B)
5.b Ternary CH refined with riding coordinates:
 C9(H9), C24(H24), C39(H39), C54(H54), C69(H69), C84(H84), C99(H99), C114(H114)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N6(H6), N8(H8), N10(H10A), N12(H12), N12A(H12A), N14(H14),
 N16(H16A), C2(H2A), C3(H3A), C4(H4A), C5(H5), C7(H7A), C11(H11), C12(H12B),
 C13(H13A), C14(H14A), C15(H15), C17(H17), C18(H18), C19(H19A), C20(H20),
 C22(H22A), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C37(H37), C41(H41), C42(H42), C43(H43), C44(H44),
  C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C56(H56),
 C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
  C67(H67), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C77(H77),
 C78(H78), C79(H79), C80(H80), C82(H82), C86(H86), C87(H87), C88(H88), C89(H89),
  C90(H90), C92(H92), C93(H93), C94(H94), C95(H95), C97(H97), C101(H101),
 C102(H102), C103(H103), C104(H104), C105(H105), C107(H107), C108(H108),
 C109(H109), C110(H110), C112(H112), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120)
5.d Idealised Me refined as rotating group:
 C121(H12C,H12D,H12E)
5.e Idealised tetrahedral OH refined as rotating group:
 O7(H7), O16(H16), O25(H25), O26(H26A)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.468
_oxdiff_exptl_absorpt_empirical_full_min 0.800