Synthesis and Properties of Donor-Acceptor-Substituted Metal-Capped Fourfold-Bridged Cyclobutadienophanes
Rolf Gleiter; Rolf Roers; Jörg Classen; Albrecht Jacobi; Gottfried Huttner; Thomas Oeser; Organometallics 19 (2000) 147–151; doi:10.1021/om9907270

data_4063204
_publ_section_title
;
 Synthesis and Properties of Donor-Acceptor-Substituted Metal-Capped
 Fourfold-Bridged Cyclobutadienophanes
;
_journal_name_full               Organometallics
_journal_page_first              147
_journal_page_last               151
_journal_paper_doi               10.1021/om9907270
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C32 H36 Co2 O2'
_chemical_formula_weight         570.47
_chemical_name_systematic
;
       
 {\h^4^:\h^4^-[3~4~]Cyclobutadienophane}(\h^5^-
 methoxycarbonylcyclopentadienyl)(\h^5^-
 cyclopentadienyl)cobalt (5)
                                 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 110.85(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   20.022(4)
_cell_length_b                   8.155(2)
_cell_length_c                   16.421(3)
_cell_measurement_temperature    200
_cell_volume                     2505.7(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       'O-Scan    '
_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  0.090
_diffrn_reflns_av_sigmaI/netI    0.062
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35851
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.353
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    'refined isotropical'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         4946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.196
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                3568
_reflns_number_total             4946
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4063204