Generation and Oligomerization ofN-Ferrocenyl Ketenimines via Open-Shell Intermediates
Kienz, Torben; Förster, Christoph; Heinze, Katja; Organometallics 35 (2016) 3681–; doi:10.1021/acs.organomet.6b00619

data_4088988
_publ_section_title
;
 Generation and Oligomerization ofN-Ferrocenyl Ketenimines via Open-Shell
 Intermediates
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3681
_journal_paper_doi               10.1021/acs.organomet.6b00619
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C72 H72 Ag6 Fe6 N6 S6'
_chemical_formula_weight         2196.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                109.710(5)
_cell_angle_beta                 106.676(4)
_cell_angle_gamma                90.193(4)
_cell_formula_units_Z            1
_cell_length_a                   9.7540(17)
_cell_length_b                   12.461(3)
_cell_length_c                   16.332(3)
_cell_measurement_reflns_used    1348
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.5007
_cell_measurement_theta_min      2.1947
_cell_volume                     1779.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1135
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8515
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.956
_diffrn_reflns_theta_min         1.747
_exptl_absorpt_coefficient_mu    3.017
_exptl_absorpt_correction_T_max  0.745638
_exptl_absorpt_correction_T_min  0.565181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.923
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8515
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+1.9574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5836
_reflns_number_total             8515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00619_si_003.cif
_cod_data_source_block           tk_119
_cod_database_code               4088988
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.570
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              28819
_shelx_hkl_checksum              6797