Chasing Weak Forces: Hierarchically Assembled Helicates as a Probe for the Evaluation of the Energetics of Weak Interactions.
Van Craen, David; Rath, Wolfgang H.; Huth, Marina; Kemp, Laura; Räuber, Christoph; Wollschläger, Jan M; Schalley, Christoph A.; Valkonen, Arto; Rissanen, Kari; Albrecht, Markus; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10098

data_4126708
_publ_section_title
;
 Chasing Weak Forces: Hierarchically Assembled Helicates as a Probe for
 the Evaluation of the Energetics of Weak Interactions.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10098
_journal_year                    2017
_chemical_formula_moiety         'C54 H48 Li3 O24 Ti2, 0.5(C18 H42 Li2 N6 O6)'
_chemical_formula_sum            'C63 H69 Li4 N3 O27 Ti2'
_chemical_formula_weight         1423.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 121.121(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.1059(15)
_cell_length_b                   22.5991(10)
_cell_length_c                   25.3240(13)
_cell_measurement_reflns_used    17087
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.0226
_cell_measurement_theta_min      3.8540
_cell_volume                     14259.9(18)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    SHELXL-2016/6
_computing_publication_material  SHELXL-2016/6
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_computing_structure_solution    'ShelXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled \w/2\t scans'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.2356
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
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_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.746
_diffrn_reflns_theta_min         2.640
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.595
_exptl_absorpt_correction_T_max  0.7325
_exptl_absorpt_correction_T_min  0.4186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       prism
_exptl_crystal_F_000             5920
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         12699
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.3142
_refine_ls_R_factor_gt           0.1260
_refine_ls_shift/su_max          0.009
_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          0.3123
_refine_ls_wR_factor_ref         0.4050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4710
_reflns_number_total             12699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10098_si_003.cif
_cod_data_source_block           Li_Ti_ethyl
_cod_original_cell_volume        14259.9(17)
_cod_database_code               4126708
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.520
_shelx_estimated_absorpt_t_max   0.638
_shelx_res_checksum              12188
_shelx_hkl_checksum              17799
_shelx_fab_checksum              75857