Combination of Spectroscopic Methods: In Situ NMR and UV/Vis Measurements To Understand the Formation of Group 4 Metallacyclopentanes from the Corresponding Metallacyclopropenes
Torsten Beweries; Christian Fischer; Stephan Peitz; Vladimir V. Burlakov; Perdita Arndt; Wolfgang Baumann; Anke Spannenberg; Detlef Heller; Uwe Rosenthal; Journal of the American Chemical Society 131 (2009) 4463–4469; doi:10.1021/ja809368s

data_4104095
_publ_section_title
;
 Combination of Spectroscopic Methods: In Situ NMR and UV/Vis Measurements
 To Understand the Formation of Group 4 Metallacyclopentanes from the
 Corresponding Metallacyclopropenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4463
_journal_page_last               4469
_journal_paper_doi               10.1021/ja809368s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C24 H32 Hf'
_chemical_formula_sum            'C24 H32 Hf'
_chemical_formula_weight         498.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.802(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7076(4)
_cell_length_b                   16.4786(7)
_cell_length_c                   12.0871(6)
_cell_measurement_reflns_used    10862
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      1.67
_cell_volume                     1892.67(15)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'rotation method'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28515
_diffrn_reflns_theta_full        26.74
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    5.515
_exptl_absorpt_correction_T_max  0.4941
_exptl_absorpt_correction_T_min  0.1442
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE (Stoe & Cie, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4014
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+0.3558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0393
_reflns_number_gt                3489
_reflns_number_total             4014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809368s_si_001.cif
_cod_data_source_block           ks694
_cod_database_code               4104095