Charge control of the inverse trans-influence
Henry S. La Pierre; Michael Rosenzweig; Boris Kosog; Christina Hauser; Frank W. Heinemann; Stephen T. Liddle; Karsten Meyer; Chem.Commun. 51 (2015) 16671–; doi:10.1039/C5cc07211E

data_7118066
_publ_section_title
;
 Charge control of the inverse trans-influence
;
_journal_name_full               Chem.Commun.
_journal_page_first              16671
_journal_paper_doi               10.1039/C5cc07211E
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety
; 
 2(C54 H87 N4 O3 Si U), C12 H30 Na O6, 3(C4 H10 O2), 3(F6 Sb)
;
_chemical_formula_sum            'C132 H234 F18 N8 Na O18 Sb3 Si2 U2'
_chemical_formula_weight         3483.75
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-08-26 deposited with the CCDC.
2015-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.9276(14)
_cell_length_b                   14.9276(14)
_cell_length_c                   63.398(11)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.69
_cell_measurement_theta_min      2.25
_cell_volume                     12234(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            65892
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    2.563
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            'violet brown'
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5292
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethoxyethane, n-hexane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 6017 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         12037
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                10156
_reflns_number_total             12037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc07211e2.cif
_cod_data_source_block           bk1014
_cod_original_sg_symbol_Hall     R3
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7118066