Enantiomerically Pure Trinuclear Helicates via Diastereoselective Self-Assembly and Characterization of Their Redox Chemistry.
Gütz, Christoph; Hovorka, Rainer; Struch, Niklas; Bunzen, Jens; Meyer-Eppler, Georg; Qu, Zheng-Wang; Grimme, Stefan; Topić, Filip; Rissanen, Kari; Cetina, Mario; Engeser, Marianne; Lützen, Arne; Journal of the American Chemical Society 136 (2014) 11830–11838; doi:10.1021/ja506327c

data_4122385
_publ_section_title
;
 Enantiomerically Pure Trinuclear Helicates via Diastereoselective
 Self-Assembly and Characterization of Their Redox Chemistry.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11830
_journal_page_last               11838
_journal_paper_doi               10.1021/ja506327c
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C258 H180 Cu3 N18 O24, 2(C5 H10 O), 6(B F4), 4(C2 H3 N)'
_chemical_formula_sum            'C276 H212 B6 Cu3 F24 N22 O26'
_chemical_formula_weight         4964.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.9576(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.0006(2)
_cell_length_b                   20.7788(3)
_cell_length_c                   43.9704(7)
_cell_measurement_reflns_used    15438
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      72.9830
_cell_measurement_theta_min      3.8960
_cell_volume                     15530.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            46538
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.750
_diffrn_reflns_theta_max         67.749
_diffrn_reflns_theta_min         3.359
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5126
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.203
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 9147 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.026(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1693
_refine_ls_number_reflns         27605
_refine_ls_number_restraints     2166
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2383
_refine_ls_wR_factor_ref         0.2650
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                22164
_reflns_number_total             27605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja506327c_si_002.cif
_cod_data_source_block           Triple_helicate
_cod_depositor_comments          'Adding full bibliography for 4122385.cif.'
_cod_database_code               4122385
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.848
_shelxl_version_number           2013-4
_shelx_res_checksum              46456
_shelx_hkl_checksum              75560
_shelx_fab_checksum              46328