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_4067795
_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         'C41 H41 Co O8'
_chemical_formula_sum            'C41 H41 Co O8'
_chemical_formula_weight         720.67
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      104
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_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            2
_cell_length_a                   15.6941(4)
_cell_length_b                   15.6941(4)
_cell_length_c                   7.2842(2)
_cell_measurement_reflns_used    4474
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      3.1
_cell_volume                     1794.13(8)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            9569
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.694
_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    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1955
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0459P)^2^+0.6240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                1704
_reflns_number_total             1955
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om200662g_si_001.cif
_cod_data_source_block           gb6_0m
_cod_database_code               4067795