Simple Synthesis of an Allenylidene Heptavalent Rhenium(d0) Complex
Xiaoyan Li; Markus Schopf; Jürgen Stephan; Jennifer Kippe; Klaus Harms; Jörg Sundermeyer; Journal of the American Chemical Society 126 (2004) 8660–8661; doi:10.1021/ja048030f

data_4112753
_publ_section_title
;
 Simple Synthesis of an Allenylidene Heptavalent Rhenium(d0) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8660
_journal_page_last               8661
_journal_paper_doi               10.1021/ja048030f
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C33 H43 N2 Re S'
_chemical_formula_weight         685.95
_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_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.787(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9538(13)
_cell_length_b                   22.3646(16)
_cell_length_c                   14.2594(13)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2.2
_cell_volume                     3172.8(6)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  IPDS
_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  0.1120
_diffrn_reflns_av_sigmaI/netI    0.1152
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21387
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    3.918
_exptl_absorpt_correction_T_max  0.7093
_exptl_absorpt_correction_T_min  0.5365
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.302
_refine_diff_density_min         -1.941
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5576
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                2705
_reflns_number_total             5576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048030fsi20040529_020722.cif
_cod_data_source_block           complex_2
_cod_database_code               4112753