Amide-Linked Heterobi- and Heterotermetallocenes with Very Low HOMO‒LUMO Gaps
Huesmann, Hannah; Förster, Christoph; Siebler, Daniel; Gasi, Teuta; Heinze, Katja; Organometallics 31 (2012) 413–; doi:10.1021/om201007g

data_4068008
_publ_section_title
;
 Amide-Linked Heterobi- and Heterotermetallocenes with Very Low HOMO--LUMO
 Gaps
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              413
_journal_paper_doi               10.1021/om201007g
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C21 H19 B2 Co F8 Fe N O'
_chemical_formula_sum            'C21 H19 B2 Co F8 Fe N O'
_chemical_formula_weight         589.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           106
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4c -2ab'
_symmetry_space_group_name_H-M   'P 42 b 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            4
_cell_length_a                   15.140(2)
_cell_length_b                   15.140(2)
_cell_length_c                   9.6200(19)
_cell_measurement_reflns_used    14784
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.69
_cell_measurement_theta_min      3.42
_cell_volume                     2205.1(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0858
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            39478
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  0.9566
_exptl_absorpt_correction_T_min  0.6629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   MULABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         2906
_refine_ls_number_restraints     1177
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+0.1603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                1639
_reflns_number_total             2906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201007g_si_002.cif
_cod_data_source_block           hh1
_cod_original_sg_symbol_H-M      P4(2)bc
_cod_database_code               4068008