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_4088026
_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         'C63 H62 N6 P2 Rh, 3 (B F4), 2 (C H2 Cl2)'
_chemical_formula_sum            'C65 H66 B3 Cl4 F12 N6 P2 Rh'
_chemical_formula_weight         1498.32
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.791(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5901(2)
_cell_length_b                   14.1532(2)
_cell_length_c                   21.0991(4)
_cell_measurement_reflns_used    16991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4650
_cell_measurement_theta_min      3.3280
_cell_volume                     3599.36(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45424
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.851
_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            colourless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.4591
_exptl_crystal_size_mid          0.1406
_exptl_crystal_size_min          0.0767
_platon_squeeze_details
; 
 PLATON: A.L. Spek, J. Appl. Cryst. 36 (2003), 7-13 
 PLATON version from 13.06.2014 
;
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.033(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         17371
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.1988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                15852
_reflns_number_total             17371
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om5b00809_si_002.cif
_cod_data_source_block           alb327sqz_8-BF4
_cod_original_cell_volume        3599.36(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4088026
_platon_squeeze_void_probe_radius 1.20