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_7701199
_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
'2(C96 H90 Dy2 N12 Na3 O24), 2(N2 O6), H2 N O4, C H4 Cl2, 3(H4 O2), O2, 2.5(C4 H6 N2)'
_chemical_formula_sum            'C203 H213 Cl2 Dy4 N34 Na6 O72'
_chemical_formula_weight         5139.90
_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            4
_cell_length_a                   20.2482(2)
_cell_length_b                   21.6632(2)
_cell_length_c                   55.8238(6)
_cell_measurement_reflns_used    28791
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      74.0980
_cell_measurement_theta_min      3.1090
_cell_volume                     24486.6(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-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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.968
_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     41.00  87.36   0.38    2.00    --    0.00  77.00 -30.00  122
  2  \w    -34.00  17.30   0.38    2.00    --    0.00  77.00 -30.00  135
  3  \w     60.00 159.18   0.38   11.00    --   95.80  82.00  60.00  261
  4  \w     47.00 120.72   0.38   11.00    --   95.80 -45.00  60.00  194
  5  \w     14.00  39.08   0.38   11.00    --   95.80 -61.00  90.00   66
  6  \w     78.00 119.80   0.38   11.00    --   95.80 -61.00  90.00  110
  7  \w     13.00 121.30   0.38   11.00    --   95.80 -45.00 -90.00  285
;
_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      0.0011185000
_diffrn_orient_matrix_UB_12      -0.0616660000
_diffrn_orient_matrix_UB_13      -0.0137409000
_diffrn_orient_matrix_UB_21      -0.0593383000
_diffrn_orient_matrix_UB_22      0.0213890000
_diffrn_orient_matrix_UB_23      -0.0151324000
_diffrn_orient_matrix_UB_31      0.0476089000
_diffrn_orient_matrix_UB_32      0.0282210000
_diffrn_orient_matrix_UB_33      -0.0185427000
_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  0.0313
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            42582
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.480
_diffrn_reflns_theta_min         3.091
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    7.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68142
_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    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             10436
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 7859 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0007(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1552
_refine_ls_number_reflns         22387
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+21.1960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_full    0.873
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                20652
_reflns_number_total             22387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02483b2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7701197--7701200.cif.'
_cod_database_code               7701199
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.68
_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
 O32-N15
 1.2 with sigma of 0.02
 N18-C101
 1.2 with sigma of 0.02
 Cl2-C103 = C103-Cl1
 1.7 with sigma of 0.02
 O31-N15 = N15-O33
 1.2 with sigma of 0.02
 O32-O31
 2.2 with sigma of 0.02
 C101-C102
 1.5 with sigma of 0.02
 H30A-H10D
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C32A) \\sim Ueq,
Uanis(C29A) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(O33)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N14, O28, O29, O30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C29, C30, C31, C32, C29A, C31A, C32A, C30A, C28A, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5)
 H31(0.5) C32(0.5) H32(0.5) O31(0.5) H31B(0.5) H31C(0.5) O32(0.5) N15(0.5)
 Cl1(0.5) O37(0.5) N17(0.5) C99(0.5) C100(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 Cl2(0.5) C28A(0.5) H28A(0.5) C29A(0.5) H29A(0.5) C30A(0.5) H30A(0.5) C31A(0.5)
 H31A(0.5) C32A(0.5) H32A(0.5) O37A(0.5) C103(0.5)
6.a Riding coordinates:
 O8(H8), O12(H12), N3(H3), O24(H24A), O31(H31B,H31C), O35(H35A,H35B), O36(H36A,
 H36B), O38(H38D,H38E), C102(H10D,H10E,H10F)
6.b Ternary CH refined with riding coordinates:
 C10(H10), C26(H26), C42(H42), C58(H58), C74(H74), C90(H90)
6.c Secondary CH2 refined with riding coordinates:
 C103(H10G,H10H)
6.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N5(H5), C2(H2), C7(H7), C8(H8A), C9(H9), C12(H12A), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C39(H39), C40(H40),
 C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), N7(H7A), N9(H9A),
 N11(H11), C50(H50), C55(H55), C56(H56), C57(H57), C60(H60), C61(H61), C62(H62),
  C63(H63), C64(H64), C66(H66), C71(H71), C72(H72), C73(H73), C76(H76),
 C77(H77), C78(H78), C79(H79), C80(H80), C82(H82), C87(H87), C88(H88), C89(H89),
  C92(H92), C93(H93), C94(H94), C95(H95), C96(H96), C28A(H28A), C29A(H29A),
 C30A(H30A), C31A(H31A), C32A(H32A)
6.e Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C22(H22A,H22B,H22C), C38(H38A,H38B,H38C), C54(H54A,H54B,
 H54C), C70(H70A,H70B,H70C), C86(H86A,H86B,H86C), C98(H98A,H98B,H98C),
 C100(H10A,H10B,H10C)
6.f Idealised tetrahedral OH refined as rotating group:
 O4(H4), O16(H16A), O20(H20)
;
_shelx_res_checksum              57004
_shelx_fab_checksum              238
_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 1.899
_oxdiff_exptl_absorpt_empirical_full_min 0.569