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_4112040
_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         'C24 H36 I3 Ru2, I3'
_chemical_formula_sum            'C24 H36 I6 Ru2'
_chemical_formula_weight         1288.07
_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           'manual editing of SHELXL template'
_cell_angle_alpha                62.1620(11)
_cell_angle_beta                 76.2329(10)
_cell_angle_gamma                73.4473(9)
_cell_formula_units_Z            2
_cell_length_a                   8.9763(5)
_cell_length_b                   14.5100(8)
_cell_length_c                   14.7824(8)
_cell_measurement_reflns_used    5686
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.400
_cell_measurement_theta_min      2.000
_cell_volume                     1619.42(16)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
'Bruker P4/RA diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\f and\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8089
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.664
_exptl_absorpt_correction_T_max  0.8251
_exptl_absorpt_correction_T_min  0.3094
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.642
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.196
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                5450
_reflns_number_total             6594
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0556023si20050823_042733_4.cif
_cod_data_source_block           18
_cod_original_cell_volume        1619.42(15)
_cod_database_code               4112040