Synthesis, Characterization, and Structural Studies of Multimetallic Ferrocenyl Carbene Complexes of Group VII Transition Metals
Daniela I. Bezuidenhout; Simon Lotz; Marilé Landman; David C. Liles; Inorganic Chemistry 50 (2011) 1521–1533; doi:10.1021/ic101784w

data_4324410
_publ_section_title
;
 Synthesis, Characterization, and Structural Studies of Multimetallic
 Ferrocenyl Carbene Complexes of Group VII Transition Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1521
_journal_page_last               1533
_journal_paper_doi               10.1021/ic101784w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C30 H28 Fe Mn2 O6'
_chemical_formula_sum            'C30 H28 Fe Mn2 O6'
_chemical_formula_weight         650.25
_chemical_name_systematic
; 
(\m~2~-(ferrocen-1,1'-diyl)-bis(ethoxy-methylidene)-C,C')-
bis(\h~5~-cyclopentadienyl-dicarbonyl-chromium) 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 118.5810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9498(11)
_cell_length_b                   9.7620(9)
_cell_length_c                   13.2618(16)
_cell_measurement_reflns_used    3770
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.185
_cell_measurement_theta_min      2.722
_cell_volume                     1358.5(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
' ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXTL and SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'SMART 1000 CCD'
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker (Seimens) P4'
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6873
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.485
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.327
_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   0.53(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0530P)^2^+0.0936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                2949
_reflns_number_total             3294
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic101784w_si_001_1.cif
_cod_data_source_block           Complex_1b
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4324410