Redox-Active Metallomacrocycles and Cyclic Metallopolymers: Photocontrolled Ring-Opening Oligomerization and Polymerization of Silicon-Bridged [1]Ferrocenophanes Using Substitutionally-Labile Lewis Bases as Initiators
David E. Herbert; Joe B. Gilroy; Wing Yan Chan; Laurent Chabanne; Anne Staubitz; Alan J. Lough; Ian Manners; Journal of the American Chemical Society 131 (2009) 14958–14968; doi:10.1021/ja904928c

data_4105146
_publ_section_title
;
 Redox-Active Metallomacrocycles and Cyclic Metallopolymers:
 Photocontrolled Ring-Opening Oligomerization and Polymerization of
 Silicon-Bridged [1]Ferrocenophanes Using Substitutionally-Labile Lewis
 Bases as Initiators
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14958
_journal_page_last               14968
_journal_paper_doi               10.1021/ja904928c
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C72 H84 Fe6 Si6'
_chemical_formula_sum            'C72 H84 Fe6 Si6'
_chemical_formula_weight         1453.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                   9.9248(14)
_cell_length_b                   9.9248(14)
_cell_length_c                   67.014(13)
_cell_measurement_reflns_used    12655
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.6
_cell_volume                     6601.0(18)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'SHELXTL V6.1'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1(Sheldrick, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       79
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            12655
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       plate
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0458P)^2^+2.3778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                3996
_reflns_number_total             5765
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja904928c_si_003.cif
_cod_data_source_block           k0742
_cod_original_cell_volume        6601.0(19)
_cod_database_code               4105146