Charge Density Analysis of the (C-C)\ρightarrowTi Agostic Interactions in a Titanacyclobutane Complex
Stephan Scheins; Marc Messerschmidt; Milan Gembicky; Mateusz Pitak; Anatoliy Volkov; Philip Coppens; Benjamin G. Harvey; Gregory C. Turpin; Atta M. Arif; Richard D. Ernst; Journal of the American Chemical Society 131 (2009) 6154–6160; doi:10.1021/ja807649k

data_4104309
_publ_section_title
;
 Charge Density Analysis of the (C-C)\\rightarrowTi Agostic Interactions
 in a Titanacyclobutane Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6154
_journal_page_last               6160
_journal_paper_doi               10.1021/ja807649k
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C17 H24 Ti'
_chemical_formula_sum            'C17 H24 Ti'
_chemical_formula_weight         276.23
_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'
_cell_angle_alpha                90
_cell_angle_beta                 99.6491(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.2455(4)
_cell_length_b                   8.17650(10)
_cell_length_c                   15.5145(3)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    90(1)
_cell_measurement_theta_max      45.294
_cell_measurement_theta_min      1.774
_cell_volume                     2907.07(8)
_computing_cell_refinement       'SMART (Bruker, 1997-2003)'
_computing_data_collection       'SMART (Bruker, 1997-2003)'
_computing_data_reduction        'SMART (Bruker, 1997-2003)'
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Bruker SMART Apex II CCD Detector
;
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            93347
_diffrn_reflns_theta_full        45.294
_diffrn_reflns_theta_max         45.294
_diffrn_reflns_theta_min         1.774
_exptl_absorpt_coefficient_mu    0.57
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.2623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1184.0
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.022
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.8177
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         11081
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0113
_refine_ls_shift/su_max          0.00000087
_refine_ls_shift/su_mean         0.0000000060
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
     calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0100
_reflns_number_gt                11081
_reflns_number_total             12643
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            ja807649k_si_001.cif
_cod_data_source_block           TIAGO
_cod_original_sg_symbol_Hall     ' -C 2yc'
_cod_database_code               4104309