d-Orbital Effects on Stereochemical Non-Rigidity: Twisted TiIV Intramolecular Dynamics
Anna V. Davis; Timothy K. Firman; Benjamin P. Hay; Kenneth N. Raymond; Journal of the American Chemical Society 128 (2006) 9484–9496; doi:10.1021/ja0617946

data_4110725
_publ_section_title
;
 d-Orbital Effects on Stereochemical Non-Rigidity: Twisted TiIV
 Intramolecular Dynamics
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9484
_journal_page_last               9496
_journal_paper_doi               10.1021/ja0617946
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C39 H54 K2 N6 O12 Ti'
_chemical_formula_sum            'C39 H54 K2 N6 O12 Ti'
_chemical_formula_weight         924.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.9569(8)
_cell_length_b                   20.9569(8)
_cell_length_c                   20.9569(8)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.38
_cell_volume                     9204.1(6)
_computing_cell_refinement       'Bruker SAINT v5.31'
_computing_data_collection       'Bruker SMART v5.052'
_computing_data_reduction        'Bruker SAINT v5.31'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      146(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       /w\2/q-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39453
_diffrn_reflns_theta_full        24.74
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9383
_exptl_absorpt_correction_T_min  0.8570
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2001'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0546
_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^)+(0.1006P)^2^+6.3831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                1959
_reflns_number_total             2626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0617946-s4.cif
_cod_data_source_block           ad5035
_cod_original_sg_symbol_Hall     '-P 2ac 2ab'
_cod_database_code               4110725