Formation of titanacyclobutenes with a spiro-bonded cyclopropane.
Shono, Tomohiro; Nagasawa, Takehiro; Tsubouchi, Akira; Noguchi, Keiichi; Takeda, Takeshi; Chemical communications (Cambridge, England)  (2008) 3537–3539; doi:10.1039/b804930k

data_7103264
_publ_section_title
;
 Formation of titanacyclobutenes with a spiro-bonded cyclopropane.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3537
_journal_page_last               3539
_journal_paper_doi               10.1039/b804930k
_journal_year                    2008
_chemical_formula_moiety         'C31 H30 Ti'
_chemical_formula_sum            'C31 H30 Ti'
_chemical_formula_weight         450.45
_chemical_name_common
;
1',1'-bis(eta5-cyclopentadienyl)-2',3'-
diphenylspiro(bicyclo(4.1.0) heptane-7,4'-(1'-titanacyclobut-2'-ene))
;
_chemical_name_systematic
;
1',1'-bis(eta5-cyclopentadienyl)-2',3'-diphenylspiro[bicyclo[4.1.0]
heptane-7,4'-(1'-titanacyclobut-2'-ene)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.7360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.34339(15)
_cell_length_b                   15.5514(3)
_cell_length_c                   17.7460(3)
_cell_measurement_reflns_used    21527
_cell_measurement_temperature    98
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.8
_cell_volume                     2262.26(7)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      98
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotaing anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30475
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    3.308
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Higashi, T. (1999). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0853P)^2^+0.4659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1786
_reflns_number_gt                3172
_reflns_number_total             4083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804930k.txt
_cod_data_source_block           I
_cod_database_code               7103264