Unprecedented Coordination Modes and Demetalation Pathways for Unbridged Polyenyl Ligands. Ruthenium η1,η4-Cycloheptadienyl Complexes from Allyl/Alkyne Cycloaddition
Christina M. Older; Robert McDonald; Jeffrey M. Stryker; Journal of the American Chemical Society 127 (2005) 14202–14203; doi:10.1021/ja0556023

data_4112039
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       jeff.stryker@ualberta.ca
_publ_contact_author_fax         +1(780)4928231
_publ_contact_author_name        'Dr Jeffrey M Stryker'
_publ_contact_author_phone       +1(780)4923891
_publ_section_title
;
 Unprecedented Coordination Modes and Demetalation Pathways for Unbridged
 Polyenyl Ligands. Ruthenium \h1,\h4-Cycloheptadienyl Complexes from
 Allyl/Alkyne Cycloaddition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14202
_journal_page_last               14203
_journal_paper_doi               10.1021/ja0556023
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C25 H35 O4 Ru, C F3 O3 S'
_chemical_formula_sum            'C26 H35 F3 O7 Ru S'
_chemical_formula_weight         649.67
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.539(2)
_cell_length_b                   17.5130(19)
_cell_length_c                   16.6622(18)
_cell_measurement_reflns_used    6168
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.369
_cell_measurement_theta_min      2.627
_cell_volume                     5409.8(10)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26192
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.8021
_exptl_absorpt_correction_T_min  0.6757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.778
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0814
_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^)+(0.0000P)^2^+48.9565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1714
_reflns_number_gt                4602
_reflns_number_total             5510
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0556023si20050823_042733_3.cif
_cod_data_source_block           14
_cod_original_cell_volume        5409.7(10)
_cod_database_code               4112039