Tight Encapsulation of a "Naked" Chloride in an Imidotitanium Hexanuclear Host
Christian Lorber; Laure Vendier; Inorganic Chemistry 52 (2013) 4756–4758; doi:10.1021/ic400211s

data_4334691
_publ_contact_author
;
Christian Lorber
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       lorber@lcc-toulouse.fr
_publ_section_title
;
 Tight Encapsulation of a "Naked" Chloride in an Imidotitanium Hexanuclear
 Host
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4756
_journal_page_last               4758
_journal_paper_doi               10.1021/ic400211s
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C72 H102 Cl13 N6 Ti6, C8 H24 N Si2, C7 H8'
_chemical_formula_sum            'C87 H134 Cl13 N7 Si2 Ti6'
_chemical_formula_weight         2082.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 120.892(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1960(11)
_cell_length_b                   17.1200(4)
_cell_length_c                   26.6290(9)
_cell_measurement_reflns_used    27208
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.2488
_cell_measurement_theta_min      3.4179
_cell_measurement_wavelength     0.71073
_cell_volume                     10639.5(8)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0159332
_diffrn_orient_matrix_UB_12      0.0091922
_diffrn_orient_matrix_UB_13      -0.0135458
_diffrn_orient_matrix_UB_21      -0.002004
_diffrn_orient_matrix_UB_22      0.0403094
_diffrn_orient_matrix_UB_23      0.0048282
_diffrn_orient_matrix_UB_31      0.0258164
_diffrn_orient_matrix_UB_32      -0.0025492
_diffrn_orient_matrix_UB_33      0.0275106
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            55633
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    0.82
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_correction_T_min  0.8451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.3
_exptl_crystal_description       block
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         21276
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+17.0717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                17746
_reflns_number_total             21276
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400211s_si_001_2.cif
_cod_data_source_block           '[*2*][(Me3Si)2NMe2]'
_cod_database_code               4334691