Synthesis, Isomerization, and Catalytic Transfer Hydrogenation Activity of Rhodium(III) Complexes Containing Both Chelating Dicarbenes and Diphosphine Ligands
Farrell, Kevin; Müller-Bunz, Helge; Albrecht, Martin; Organometallics 34 (2015) 5723–; doi:10.1021/acs.organomet.5b00809

data_4088024
_publ_section_title
;
 Synthesis, Isomerization, and Catalytic Transfer Hydrogenation Activity
 of Rhodium(III) Complexes Containing Both Chelating Dicarbenes and
 Diphosphine Ligands
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5723
_journal_paper_doi               10.1021/acs.organomet.5b00809
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C45 H54 N6 P2 Rh, 3 (B F4), C H2 Cl2, C2 H3 N'
_chemical_formula_sum            'C48 H59 B3 Cl2 F12 N7 P2 Rh'
_chemical_formula_weight         1230.20
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.9400(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3773(1)
_cell_length_b                   24.0260(3)
_cell_length_c                   16.9704(2)
_cell_measurement_reflns_used    38777
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.7990
_cell_measurement_theta_min      3.7810
_cell_volume                     5402.05(10)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56155
_diffrn_reflns_theta_full        76.80
_diffrn_reflns_theta_max         76.80
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    4.754
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24a (release 19-12-2012 CrysAlis171 .NET) 
(compiled Dec 19 2012,11:08:27) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.2692
_exptl_crystal_size_mid          0.1687
_exptl_crystal_size_min          0.0436
_platon_squeeze_details
; 
 PLATON: A.L. Spek, J. Appl. Cryst. 36 (2003), 7-13 
 PLATON version from 27.07.2012 
;
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         10595
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+11.9762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                10451
_reflns_number_total             10595
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om5b00809_si_002.cif
_cod_data_source_block           alb232sqz_6a
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4088024