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_4063203
_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            'C34 H38 Co2 O4'
_chemical_formula_weight         628.5
_chemical_name_systematic
; 
 {\h^4^:\h^4^-[3~4~]Cyclobutadienophane}bis(\h^5^-
 methoxycarbonylcyclopentadienyl)cobalt (2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                90.0
_cell_angle_beta                 107.96(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   9.595(2)
_cell_length_b                   13.832(4)
_cell_length_c                   10.998(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.0
_cell_measurement_theta_min      10.2
_cell_volume                     1388.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  NONIUS_CAD4
_diffrn_measurement_method       \w2\q-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  0.037
_diffrn_reflns_av_sigmaI/netI    0.024
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3534
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.23
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.50
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.035
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+0.1290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.092
_refine_ls_wR_factor_ref         0.099
_reflns_number_gt                2753
_reflns_number_total             3345
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4063203