New and Selective Routes to Functionalized Biferrocenes and Terferrocenes by [3 + 2] Cycloadditions of Alkynes with Bridging C3Ligands in Diiron Complexes
Salmi, Mauro; Busetto, Luigi; Mazzoni, Rita; Zacchini, Stefano; Zanotti, Valerio; Organometallics 30 (2011) 1175–; doi:10.1021/om101162r

data_4064152
_publ_section_title
;
 New and Selective Routes to Functionalized Biferrocenes and Terferrocenes
 by [3 + 2] Cycloadditions of Alkynes with Bridging C3Ligands in Diiron
 Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1175
_journal_paper_doi               10.1021/om101162r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C31 H27 Cl3 Fe3'
_chemical_formula_weight         673.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   18.391(2)
_cell_length_b                   20.224(3)
_cell_length_c                   7.7205(10)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.175
_cell_measurement_theta_min      2.215
_cell_volume                     2871.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14125
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.7384
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.050(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         2924
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0186
_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^)+(0.0248P)^2^+0.8472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                2833
_reflns_number_total             2924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101162r_si_001.cif
_cod_data_source_block           cmc21
_cod_original_cell_volume        2871.5(6)
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               4064152