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_4088989
_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            'C37 H39 Cl2 F12 Fe3 N3 S Sb2'
_chemical_formula_weight         1267.72
_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                104.403(2)
_cell_angle_beta                 92.447(2)
_cell_angle_gamma                96.711(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6219(8)
_cell_length_b                   13.1000(11)
_cell_length_c                   17.2736(15)
_cell_measurement_temperature    173(2)
_cell_volume                     2088.6(3)
_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 0.995
_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_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.1236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24230
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.007
_diffrn_reflns_theta_min         1.761
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_T_max  1.14058
_exptl_absorpt_correction_T_min  0.86244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   MULABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.535
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         10047
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5616
_reflns_number_total             10047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00619_si_004.cif
_cod_data_source_block           tk6
_cod_database_code               4088989
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.656
_shelx_estimated_absorpt_t_max   0.905
_exptl_absorpt_special_details   MULABS
_shelx_res_checksum              12706
_shelx_hkl_checksum              37802