An Improved Protocol for the Synthesis of [(η4-C4R4)Co(η5-C5H5)] Complexes
Bertrand, Guillaume; Tortech, Ludovic; Fichou, Denis; Malacria, Max; Aubert, Corinne; Gandon, Vincent; Organometallics 31 (2012) 126–; doi:10.1021/om200662g

data_4067797
_publ_section_title
;
 An Improved Protocol for the Synthesis of [(\h4-C4R4)Co(\h5-C5H5)]
 Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              126
_journal_paper_doi               10.1021/om200662g
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C57 H41 Co'
_chemical_formula_sum            'C57 H41 Co'
_chemical_formula_weight         784.83
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.45(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.906(11)
_cell_length_b                   11.782(7)
_cell_length_c                   22.282(13)
_cell_measurement_reflns_used    5278
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.5
_cell_volume                     4687(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND. Crystal Impact GbR, Bonn, Germany'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            50477
_diffrn_reflns_theta_full        27.77
_diffrn_reflns_theta_max         27.76
_diffrn_reflns_theta_min         2.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1461P)^2^+1.0385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2260
_reflns_number_gt                7485
_reflns_number_total             10785
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om200662g_si_003.cif
_cod_data_source_block           gb12_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4067797