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_4064888
_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         'C27 H26 Fe O2 Ru'
_chemical_formula_sum            'C27 H26 Fe O2 Ru'
_chemical_formula_weight         539.40
_chemical_melting_point          494.1(10)
_chemical_name_common            '[Ru(Cp*){1,2-C5H3(CO)2-1,2-C5H3)}Fe(Cp)]'
_chemical_name_systematic
'[Ru(Cp*){m2-h5:h5-1,2-C5H3(CO)2-1,2-C5H3)}Fe(Cp)]'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 92.167(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3554(3)
_cell_length_b                   11.1759(5)
_cell_length_c                   12.9896(5)
_cell_measurement_reflns_used    4731
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.04
_cell_measurement_theta_min      5.22
_cell_volume                     1067.02(8)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker-AXS, 2006)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
; 
SHELX-97 (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 5.6
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17341
_diffrn_reflns_theta_full        68.37
_diffrn_reflns_theta_max         68.37
_diffrn_reflns_theta_min         3.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.350
_exptl_absorpt_correction_T_max  0.467
_exptl_absorpt_correction_T_min  0.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs in APEX2 (BrukerAXS, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.186
_refine_diff_density_min         -2.479
_refine_diff_density_rms         0.232
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         1965
_refine_ls_number_restraints     421
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0665
_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^)+(0.1398P)^2^+9.3621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1958
_refine_ls_wR_factor_ref         0.1960
_reflns_number_gt                1952
_reflns_number_total             1965
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om2003915_si_002.cif
_cod_data_source_block           x10080
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '220-222 C' was changed to
'494.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4064888