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_4324412
_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         'C40 H18 Fe O20 Re4 Ti, 2(H2 O)'
_chemical_formula_sum            'C40 H22 Fe O22 Re4 Ti'
_chemical_formula_weight         1703.13
_chemical_name_systematic
; 
(\m~2~-(1,1'-ferrocenyl)-bis((nonacarbonyl)-dirhenium-oxy-methylidene)-O,O')-
bis(\h^5^-cyclopentadienyl)-titanium dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.9060(10)
_cell_angle_beta                 94.7320(10)
_cell_angle_gamma                95.6650(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7406(7)
_cell_length_b                   12.1924(8)
_cell_length_c                   18.4356(12)
_cell_measurement_reflns_used    5348
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.331
_cell_measurement_theta_min      2.607
_cell_volume                     2393.5(3)
_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 (The POV-Ray Team, 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 0.972
_diffrn_measured_fraction_theta_max 0.879
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12826
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    10.607
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    2.363
_exptl_crystal_description       square-plate
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.273
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.246
_refine_ls_extinction_coef       0.00036(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         8569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0781P)^2^+19.0868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                6203
_reflns_number_total             8569
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic101784w_si_001_3.cif
_cod_data_source_block           Complex_4b
_cod_database_code               4324412