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_4110726
_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         'C54 H82 N10 Na2 O16 Ti, C3 H7 N O'
_chemical_formula_sum            'C57 H89 N11 Na2 O17 Ti'
_chemical_formula_weight         1294.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 106.161(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8619(12)
_cell_length_b                   17.1753(12)
_cell_length_c                   22.8947(16)
_cell_measurement_reflns_used    4185
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      2.24
_cell_volume                     6746.2(8)
_computing_cell_refinement       'Bruker SAINT v5.01'
_computing_data_collection       'Bruker SMART v5.052'
_computing_data_reduction        'Bruker SAINT v5.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14817
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.9689
_exptl_absorpt_correction_T_min  0.9411
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2001'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+6.2506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                3956
_reflns_number_total             5555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0617946-s5.cif
_cod_data_source_block           ad5107
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4110726