Structural Consequences of Anionic Host-Cationic Guest Interactions in a Supramolecular Assembly
Michael D. Pluth; Darren W. Johnson; Géza Szigethy; Anna V. Davis; Simon J. Teat; Allen G. Oliver; Robert G. Bergman; Kenneth N. Raymond; Inorganic Chemistry 48 (2009) 111–120; doi:10.1021/ic8012848

data_4301074
_publ_section_title
;
Structural Consequences of Anionic Host-Cationic Guest Interactions in a
Supramolecular Assembly
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              111
_journal_page_last               120
_journal_paper_doi               10.1021/ic8012848
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
;
'C182 H111 N17.50 O36 Ti4' 
;
_chemical_formula_sum            'C182 H111 N17.5 O36 Ti4'
_chemical_formula_weight         3310.48
_chemical_melting_point          ?
_chemical_name_common            'Ti4L6 Et4N cluster'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   20.844(3)
_cell_length_b                   20.844(3)
_cell_length_c                   163.55(5)
_cell_measurement_reflns_used    7627
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.045
_cell_measurement_theta_min      2.256
_cell_volume                     61538(2)
_computing_cell_refinement       'Bruker SAINT v.7.23'
_computing_data_collection       'Bruker APEX2 v.2.0.2'
_computing_data_reduction        'Bruker SATIN v.7.23'
_computing_molecular_graphics    'ORTEP-3 v.1.08, POV-Ray v.3.6.1c.icl8.win32'
_computing_publication_material  'ORTEP-3 v.1.08, POV-Ray v.3.6.1c.icl8.win32'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 3.623
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Platinum 200'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'channel cut Si-(111) crystal'
_diffrn_radiation_source         'Advanced Light Source Station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       138
_diffrn_reflns_limit_l_min       -133
_diffrn_reflns_number            48435
_diffrn_reflns_theta_full        19.32
_diffrn_reflns_theta_max         19.32
_diffrn_reflns_theta_min         1.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.9579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'trigonal prism'
_exptl_crystal_F_000             20418
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         4345
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      2.099
_refine_ls_R_factor_all          0.1703
_refine_ls_R_factor_gt           0.1594
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4533
_refine_ls_wR_factor_ref         0.4669
_reflns_number_gt                3636
_reflns_number_total             4345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8012848_si_002_1.cif
_cod_data_source_block           Structure3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        61540(25)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C182 H111 N17.50 O36 Ti4'
_cod_database_code               4301074