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_4112037
_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         'C23 H31 O4 Ru, F6 P'
_chemical_formula_sum            'C23 H31 F6 O4 P Ru'
_chemical_formula_weight         617.52
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   22.4394(6)
_cell_length_b                   8.6159(4)
_cell_length_c                   12.8730(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      29.37
_cell_measurement_theta_min      28.90
_cell_volume                     2488.81(15)
_computing_cell_refinement       'Siemens XSCANS (Siemens, 1996)'
_computing_data_collection       'Siemens XSCANS (Siemens, 1996)'
_computing_data_reduction        'Siemens SHELXTL (Siemens, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL (Siemens, 1997)'
_computing_publication_material  'Siemens SHELXTL (Siemens, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Siemens P4/RA'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3485
_diffrn_reflns_theta_full        56.75
_diffrn_reflns_theta_max         56.75
_diffrn_reflns_theta_min         3.94
_diffrn_standards_decay_%        12.36
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.376
_exptl_absorpt_correction_T_max  0.2507
_exptl_absorpt_correction_T_min  0.1219
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Siemens SHELXTL (Siemens, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         3312
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0715P)^2^+2.2524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                3195
_reflns_number_total             3312
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0556023si20050823_042733_1.cif
_cod_data_source_block           12
_cod_database_code               4112037