Preparation and Crystallographic Characterization of C60{η(1)-Ru(CO)2(η(5)-C5H5)}2: A Locally Crowded Organometallic Fullerene Without the Usual η(2)-Bonding.
Bowles, Faye L.; Olmstead, Marilyn M.; Balch, Alan L.; Journal of the American Chemical Society 136 (2014) 3338–3341; doi:10.1021/ja4120677

data_4121504
_publ_section_title
;
 Preparation and Crystallographic Characterization of
 C60{\h(1)-Ru(CO)2(\h(5)-C5H5)}2: A Locally Crowded Organometallic
 Fullerene Without the Usual \h(2)-Bonding.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3338
_journal_page_last               3341
_journal_paper_doi               10.1021/ja4120677
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C74 H10 O4 Ru2'
_chemical_formula_sum            'C74 H10 O4 Ru2'
_chemical_formula_weight         1164.96
_chemical_name_common
'Bis-cyclopentadienylruthenium dicarbonyl[C60]fullerene'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.28(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.408(3)
_cell_length_b                   13.224(3)
_cell_length_c                   20.014(4)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.728
_cell_measurement_theta_min      2.245
_cell_volume                     3952.0(15)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2004 (Burla et al., 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            64292
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         38.775
_diffrn_reflns_theta_min         1.487
_diffrn_source                   'Advanced Light Source, Beamline 11.3.1'
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.024
_exptl_crystal_size_mid          0.009
_exptl_crystal_size_min          0.004
_refine_diff_density_max         2.315
_refine_diff_density_min         -2.119
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1142
_refine_ls_number_reflns         17211
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+10.4403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15519
_reflns_number_total             17211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4120677_si_002.cif
_cod_data_source_block           fb35
_cod_database_code               4121504
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2013-4
_shelx_res_checksum              33163
_shelx_hkl_checksum              84072