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_7232339
_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 unk
_chemical_formula_moiety         'C42 H30 Dy2 N6 O14, 4(O)'
_chemical_formula_sum            'C42 H42 Dy2 N6 O18'
_chemical_formula_weight         1243.82
_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                   17.5291(14)
_cell_length_b                   17.5291(14)
_cell_length_c                   14.569(2)
_cell_measurement_reflns_used    13032
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4476.6(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 50.2822
              2theta: 29.8528
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 120.0000
                 XTD: 50.2822
              2theta: 29.8528
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 240.0000
                 XTD: 50.2822
              2theta: 29.8528
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.031722
_diffrn_orient_matrix_UB_12      0.006168
_diffrn_orient_matrix_UB_13      -0.047012
_diffrn_orient_matrix_UB_21      -0.041622
_diffrn_orient_matrix_UB_22      0.023471
_diffrn_orient_matrix_UB_23      0.031164
_diffrn_orient_matrix_UB_31      0.027326
_diffrn_orient_matrix_UB_32      0.062119
_diffrn_orient_matrix_UB_33      -0.010288
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17905
_diffrn_reflns_point_group_measured_fraction_full 0.842
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         3.028
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.396
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 2248 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         6651
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.621
_reflns_Friedel_fraction_full    0.675
_reflns_Friedel_fraction_max     0.675
_reflns_number_gt                6407
_reflns_number_total             6651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01242c2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7232339--7232346.cif.
;
_cod_original_cell_volume        4476.6(10)
_cod_database_code               7232339
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.550
_shelx_estimated_absorpt_t_min   0.550
_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
N5 \\sim C37 \\sim C35 \\sim C34 \\sim C36: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
O15 \\sim C14 \\sim C13 \\sim C10 \\sim C9 \\sim N2: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.01
O17 \\sim O18 \\sim O5 \\sim C15 \\sim C16 \\sim C22 \\sim C21 \\sim N3 \\sim
C23 \\sim C24: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.01
O16 \\sim N1 \\sim C7 \\sim C8 \\sim C2 \\sim C1: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.01
O18 \\sim O17 \\sim O16 \\sim O15: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C37(H37A,H37B), C23(H23A,H23B)
3.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C20(H20), C17(H17), N1(H1), N3(H3), C6(H6), C3(H3A), C8(H8), C36(H36),
  C31(H31), C34(H34), C25(H25), C22(H22), C11(H11), C14(H14), C27(H27),
 C13(H13), C26(H26), C41(H41), C39(H39), C28(H28), C12(H12), C42(H42), C40(H40)
;
_olex2_submission_special_instructions 'No special instructions were received'