Ruthenocene 1,2-Dicarboxylic Acid, Carboxylic Anhydride, and Acid Chloride: A Facile Route to Metallocene-Fused Acenequinones
Pokharel, Uttam Raj; Selegue, John P.; Parkin, Sean; Organometallics 30 (2011) 3254–; doi:10.1021/om2003915

data_4064885
_publ_section_title
;
 Ruthenocene 1,2-Dicarboxylic Acid, Carboxylic Anhydride, and Acid
 Chloride: A Facile Route to Metallocene-Fused Acenequinones
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3254
_journal_paper_doi               10.1021/om2003915
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C17 H20 O4 Ru, 0.362(C H4 O)'
_chemical_formula_sum            'C17.36 H21.44 O4.36 Ru'
_chemical_formula_weight         400.98
_chemical_melting_point          '210-230 C (dec)'
_chemical_name_common            '[Ru{C5H3(COOH)2-1,2}(Cp*)]'
_chemical_name_systematic        '[Ru{C5H3(COOH)2-1,2}(Cp*)]'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3634(7)
_cell_length_b                   14.8024(8)
_cell_length_c                   15.3413(8)
_cell_measurement_reflns_used    9557
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.62
_cell_measurement_theta_min      2.88
_cell_volume                     3261.8(3)
_computing_cell_refinement       'APEX2 (Bruker-AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2006)'
_computing_data_reduction        'APEX2 (Bruker-AXS, 2006)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
; 
SHELX97-2 (Sheldrick, 2008) and local procedures 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker X8 Proteum diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graded multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47731
_diffrn_reflns_theta_full        68.73
_diffrn_reflns_theta_max         68.73
_diffrn_reflns_theta_min         4.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.947
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs in APEX2 (BrukerAXS, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1636.1
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.258(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+4.0957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0607
_reflns_number_gt                5939
_reflns_number_total             5989
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om2003915_si_002.cif
_cod_data_source_block           x08101
_cod_database_code               4064885