Coordination complexes of bivalent ansa-ytterbocenes: synthesis, structure and comparison with related unbridged ytterbocenes and ansa-ferrocenes
Schultz, Madeleine; Sofield, Chadwick D.; Walter, Marc D.; Andersen, Richard A.; New Journal of Chemistry 29 (2005) 919–; doi:10.1039/b418550a

data_7050076
_publ_section_title
;
 Coordination complexes of bivalent ansa-ytterbocenes: synthesis,
 structure and comparison with related unbridged ytterbocenes and
 ansa-ferrocenes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              919
_journal_paper_doi               10.1039/b418550a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C24 H46 Fe Si5'
_chemical_formula_sum            'C24 H46 Fe Si5'
_chemical_formula_weight         530.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 96.8100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.5073(2)
_cell_length_b                   12.06730(10)
_cell_length_c                   32.66810(10)
_cell_measurement_reflns_used    7758
_cell_measurement_temperature    159(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2
_cell_volume                     6070.09(10)
_computing_cell_refinement       'Bruker SAINT V. 6.40'
_computing_data_collection       'Bruker SMART V. 5.0.54D'
_computing_data_reduction        'Bruker SAINT V. 6.40'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      159(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \w-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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            12365
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.8837
_exptl_absorpt_correction_T_min  0.8060
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+12.6429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                3812
_reflns_number_total             4353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418550a.txt
_cod_data_source_block           ansafem
_cod_original_cell_volume        6070.09(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050076