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_4112038
_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         'C27 H39 O4 Ru, C24 H20 B, 2(C H2 Cl2)'
_chemical_formula_sum            'C51 H59 B Cl4 O4 Ru'
_chemical_formula_weight         989.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90.00
_cell_angle_beta                 92.46(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.779(2)
_cell_length_b                   19.272(6)
_cell_length_c                   21.152(7)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      12.75
_cell_measurement_theta_min      8.95
_cell_volume                     4797(2)
_computing_cell_refinement       'CAD4/PC (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/PC (Enraf-Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL (Siemens, 1997)'
_computing_publication_material  'Siemens SHELXTL (Siemens, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_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_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6917
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.0
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.886
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6729
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1983
_refine_ls_R_factor_gt           0.0975
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+25.3668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2685
_refine_ls_wR_factor_ref         0.2227
_reflns_number_gt                3195
_reflns_number_total             6729
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0556023si20050823_042733_2.cif
_cod_data_source_block           13
_cod_original_cell_volume        4797.4(24)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4112038