Operationally Unsaturated Pincer/Rhenium Complexes Form Metal Carbenes from Cycloalkenes and Metal Carbynes from Alkanes
Oleg V. Ozerov; Lori A. Watson; Maren Pink; Kenneth G. Caulton; Journal of the American Chemical Society 129 (2007) 6003–6016; doi:10.1021/ja062327r

data_4109368
_publ_section_title
;
 Operationally Unsaturated Pincer/Rhenium Complexes Form Metal Carbenes
 from Cycloalkenes and Metal Carbynes from Alkanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6003
_journal_page_last               6016
_journal_paper_doi               10.1021/ja062327r
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C32.5 H64 N P2 Re Si2'
_chemical_formula_weight         773.17
_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                103.6860(10)
_cell_angle_beta                 103.8770(10)
_cell_angle_gamma                101.6850(10)
_cell_formula_units_Z            4
_cell_length_a                   11.3353(3)
_cell_length_b                   18.1292(6)
_cell_length_c                   18.4996(6)
_cell_measurement_reflns_used    9513
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.32
_cell_volume                     3447.78(19)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      111(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'   0.30 degree frames measured for  10.14 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w 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  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            94882
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.18
_diffrn_standards_interval_time  614
_exptl_absorpt_coefficient_mu    3.709
_exptl_absorpt_correction_T_max  0.8362
_exptl_absorpt_correction_T_min  0.3568
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         20095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.339
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+3.0671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                15501
_reflns_number_total             20095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja062327rrom20060411_023842.cif
_cod_data_source_block           d:\2001data\01114lb\sad
_cod_original_cell_volume        3447.78(18)
_cod_original_formula_sum        'C32.50 H64 N P2 Re Si2'
_cod_database_code               4109368