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_4088103
_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         'C21 H26 Cl Fe O Rh'
_chemical_formula_sum            'C21 H26 Cl Fe O Rh'
_chemical_formula_weight         488.63
_chemical_name_systematic
;
 Chloro-(\h^4^-1,5-cyclooctadienyl)-(ferrocenyl-ethoxy-carbene)-rhodium
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/5
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1117(3)
_cell_length_b                   15.6717(7)
_cell_length_c                   17.0417(8)
_cell_measurement_reflns_used    9499
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      38.439
_cell_measurement_theta_min      2.390
_cell_volume                     1899.34(15)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_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      120(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0609
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            120529
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.470
_diffrn_reflns_theta_min         2.390
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.119
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 4470 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.502(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         12080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0290P)^2^+1.2534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                10819
_reflns_number_total             12080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00843_si_002.cif
_cod_data_source_block           KB053LT_Complex_1
_cod_database_code               4088103
_shelx_estimated_absorpt_t_min   0.612
_shelx_estimated_absorpt_t_max   0.816
_shelxl_version_number           2014/5
_shelx_res_checksum              64564
_shelx_hkl_checksum              69856