Self-selecting homochiral quadruple-stranded helicates and control of supramolecular chirality.
Boer, Stephanie A.; Turner, David R.; Chemical communications (Cambridge, England) 51 (2015) 17375–17378; doi:10.1039/c5cc07422c

data_7118132
_publ_section_title
;
 Self-selecting homochiral quadruple-stranded helicates and control of
 supramolecular chirality.
;
_journal_issue                   98
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              17375
_journal_page_last               17378
_journal_paper_doi               10.1039/c5cc07422c
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C116 H108 D12 Cu4 N8 O44 S6, 2(C2 D6 O S)'
_chemical_formula_sum            'C120 H108 Cu4 D24 N8 O46 S8'
_chemical_formula_weight         2957.12
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-03 deposited with the CCDC.
2015-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                72.648(7)
_cell_angle_beta                 65.229(3)
_cell_angle_gamma                89.532(12)
_cell_formula_units_Z            1
_cell_length_a                   15.638(3)
_cell_length_b                   15.8320(6)
_cell_length_c                   18.4820(19)
_cell_measurement_reflns_used    101474
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.960
_cell_measurement_theta_min      1.456
_cell_volume                     3929.5(9)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            101474
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.960
_diffrn_reflns_theta_min         1.456
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
Voids 2 and 6 are within the cage, all others are between cages.
2 + 6 calculate to approx. 3 DMSO molecules or 18 water molecules.
Concordant analysis difficult to obtain with certainty.
;
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 12502 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.046(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1808
_refine_ls_number_reflns         36907
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1800P)^2^+1.4427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2555
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                30085
_reflns_number_total             36907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc07422c2.cif
_cod_data_source_block           dmso_sq
_cod_database_code               7118132
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              92015
_shelx_hkl_checksum              84821
_shelx_fab_checksum              97487