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_4088987
_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            'C76 H86 B2 Cl8 Cu2 F8 Fe6 N6 S6'
_chemical_formula_weight         2195.27
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                60.772(6)
_cell_angle_beta                 71.684(6)
_cell_angle_gamma                78.348(6)
_cell_formula_units_Z            1
_cell_length_a                   11.092(3)
_cell_length_b                   15.327(4)
_cell_length_c                   15.563(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2188.2(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.1713
_diffrn_reflns_av_sigmaI/netI    0.3279
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21797
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    1.891
_exptl_absorpt_correction_T_max  0.8048
_exptl_absorpt_correction_T_min  0.5492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   MULABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         10513
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.2343
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                3560
_reflns_number_total             10513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00619_si_002.cif
_cod_data_source_block           tk5
_cod_original_cell_volume        2188.3(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4088987