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_4110724
_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         'C51 H72 Ge K2 N6 O15, C3 H6 O'
_chemical_formula_sum            'C54 H78 Ge K2 N6 O16'
_chemical_formula_weight         1218.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.074(2)
_cell_angle_beta                 75.986(2)
_cell_angle_gamma                80.030(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4117(14)
_cell_length_b                   13.7070(15)
_cell_length_c                   19.505(2)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    166(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.47
_cell_volume                     3169.8(6)
_computing_cell_refinement       'Bruker SINT v5.01'
_computing_data_collection       'Bruker SMART v5.052'
_computing_data_reduction        'Bruker SINT v5.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      166(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18498
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.8759
_exptl_absorpt_correction_T_min  0.7272
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.547
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         10716
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+3.9986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                9060
_reflns_number_total             10716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0617946-s3.cif
_cod_data_source_block           ad6145
_cod_original_cell_volume        3169.9(6)
_cod_database_code               4110724