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_4088106
_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         'C32 H29 Cl Fe O2 P Rh, 2(C H2 Cl2)'
_chemical_formula_sum            'C34 H33 Cl5 Fe O2 P Rh'
_chemical_formula_weight         840.58
_chemical_name_systematic
;
 Chloro-carbonyl-(triphenylphosphine)-(ferrocenyl-n-propylamino-carbene)
-rhodium bis(dichloromethane) solvate
;
_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
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                83.776(3)
_cell_angle_beta                 88.267(3)
_cell_angle_gamma                71.216(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1692(6)
_cell_length_b                   13.2020(8)
_cell_length_c                   13.6942(8)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.282
_cell_measurement_theta_min      2.221
_cell_volume                     1730.30(18)
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_collection       'APEX2 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_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, PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL, SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7590
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular-fragment
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0670
_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^)+(0.1525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                6226
_reflns_number_total             7590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00843_si_002.cif
_cod_data_source_block           KB082x2_Complex_5
_cod_database_code               4088106
_shelx_estimated_absorpt_t_min   0.599
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              88394
_shelx_hkl_checksum              95469