Formation of {Co(dppe)}2{μ2-η(2):η(2)-η(2):η(2)-[(C60)2]} Dimers Bonded by Single C-C Bonds and Bridging η(2)-Coordinated Cobalt Atoms.
Konarev, Dmitri V.; Troyanov, Sergey I.; Ustimenko, Kseniya A.; Nakano, Yoshiaki; Shestakov, Alexander F.; Otsuka, Akihiro; Yamochi, Hideki; Saito, Gunzi; Lyubovskaya, Rimma N.; Inorganic chemistry 54 (2015) 4597–4599; doi:10.1021/acs.inorgchem.5b00637

data_4342918
_publ_section_title
;
 Formation of {Co(dppe)}2{\m2-\h(2):\h(2)-\h(2):\h(2)-[(C60)2]} Dimers
 Bonded by Single C-C Bonds and Bridging \h(2)-Coordinated Cobalt Atoms.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4597
_journal_page_last               4599
_journal_paper_doi               10.1021/acs.inorgchem.5b00637
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '(C172 H48 Co2 P4), 3(C6 H4 Cl2)'
_chemical_formula_sum            'C190 H60 Cl6 Co2 P4'
_chemical_formula_weight         2796.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                99.756(5)
_cell_angle_beta                 93.345(9)
_cell_angle_gamma                102.701(8)
_cell_formula_units_Z            2
_cell_length_a                   17.145(1)
_cell_length_b                   17.552(1)
_cell_length_c                   19.776(1)
_cell_measurement_reflns_used    38000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     5693.2(6)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXD
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_device_type  MAR225
_diffrn_measurement_method       CCD
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.81036
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_laue_measured_fraction_full 0.904
_diffrn_reflns_laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            104876
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        28.800
_diffrn_reflns_theta_max         34.793
_diffrn_reflns_theta_min         1.395
_diffrn_source                   'BL 14.2 PSF, BESSY, Berlin, Germany'
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       plate
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.194
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2307
_refine_ls_number_reflns         27263
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+19.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24261
_reflns_number_total             27263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00637_si_002.cif
_cod_data_source_block           CODPPE
_cod_depositor_comments          'Adding full bibliography for 4342918.cif.'
_cod_database_code               4342918
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              73268
_shelx_hkl_checksum              50995