Unprecedented homochiral 3D lanthanide coordination polymers with triple-stranded helical architecture constructed from a rigid achiral aryldicarboxylate ligand
You, Li-Xin; Xie, Shi-Yu; Xia, Cheng-Cai; Wang, Shu-Ju; Xiong, Gang; He, Yong-Ke; Dragutan, Ileana; Dragutan, Valerian; Fedin, Vladimir P.; Sun, Ya-Guang; CrystEngComm 21 (2019) 1758–; doi:10.1039/C8CE01242C

data_7232343
_publ_section_title
;
 Unprecedented homochiral 3D lanthanide coordination polymers with
 triple-stranded helical architecture constructed from a rigid achiral
 aryldicarboxylate ligand
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1758
_journal_paper_doi               10.1039/C8CE01242C
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C42 H30 N6 O14 Yb2, 4(O)'
_chemical_formula_sum            'C42 H42 N6 O18 Yb2'
_chemical_formula_weight         1264.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-07 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4158(6)
_cell_length_b                   17.4158(6)
_cell_length_c                   14.4403(9)
_cell_measurement_reflns_used    13583
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4379.9(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 49.9979
              2theta: 29.9451
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 120.0000
                 XTD: 49.9979
              2theta: 29.9451
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 240.0000
                 XTD: 49.9979
              2theta: 29.9451
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.008906
_diffrn_orient_matrix_UB_12      0.009215
_diffrn_orient_matrix_UB_13      0.055971
_diffrn_orient_matrix_UB_21      -0.055305
_diffrn_orient_matrix_UB_22      0.011184
_diffrn_orient_matrix_UB_23      -0.010642
_diffrn_orient_matrix_UB_31      -0.015208
_diffrn_orient_matrix_UB_32      -0.067009
_diffrn_orient_matrix_UB_33      0.008613
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26289
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.004
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_min         3.054
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.330
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.064
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 3476 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(8)
_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     613
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     1669
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0423P)^2^+1.7601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                7468
_reflns_number_total             7626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01242c2.cif
_cod_data_source_block           shelx_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7232339--7232346.cif.'
_cod_original_cell_volume        4379.9(4)
_cod_database_code               7232343
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.478
_shelx_estimated_absorpt_t_min   0.478
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.01
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C37(H37A,H37B), C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), N1(H1), C5(H5), C25(H25), C16(H16), C13(H13), C11(H11),
 N2(H2), C35(H35), C31(H31), C26(H26), N4(H4), C28(H28), C27(H27), C22(H22),
 C41(H41), C42(H42), C19(H19), C21(H21), C20(H20), C39(H39), C40(H40), C33(H33)
;
_olex2_submission_special_instructions 'No special instructions were received'