Rhodium(I) Ferrocenylcarbene Complexes: Synthesis, Structural Determination, Electrochemistry, and Application as Hydroformylation Catalyst Precursors
Ramollo, G. Kabelo; López-Gómez, María J.; Liles, David C.; Matsinha, Leah C.; Smith, Gregory S.; Bezuidenhout, Daniela I.; Organometallics 34 (2015) 5745–; doi:10.1021/acs.organomet.5b00843

data_4088105
_publ_section_title
;
 Rhodium(I) Ferrocenylcarbene Complexes: Synthesis, Structural
 Determination, Electrochemistry, and Application as Hydroformylation
 Catalyst Precursors
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5745
_journal_paper_doi               10.1021/acs.organomet.5b00843
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C16 H17 Cl Fe N O2 Rh'
_chemical_formula_sum            'C16 H17 Cl Fe N O2 Rh'
_chemical_formula_weight         449.51
_chemical_name_systematic
;
 Dicarbonyl-chloro-(ferrocenyl-propylamino-carbene)-rhodium
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.669(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2379(5)
_cell_length_b                   11.6398(4)
_cell_length_c                   15.4055(9)
_cell_measurement_reflns_used    54063
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.97
_cell_volume                     1653.12(14)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT program (Nonius, 2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
 ORTEP-3 for Windows (Farrugia, 1997), POV-RAY (Cason, 2004),
 Mercury (Macrae <i>et al</i>., 2008)
;
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '1.0\% \f scans and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54063
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         3.966
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_transmission_factor_max   0.946
_exptl_transmission_factor_min   0.820
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3758
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0242P)^2^+1.2846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                3366
_reflns_number_total             3758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00843_si_002.cif
_cod_data_source_block           KB111_Complex_4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088105
_shelx_estimated_absorpt_t_min   0.686
_shelx_estimated_absorpt_t_max   0.777
_shelx_res_checksum              81165
_shelx_hkl_checksum              98920