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_4088023
_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 N5 P2 Rh, 2 (B F4), 2 (C H2 Cl2)'
_chemical_formula_sum            'C47 H58 B2 Cl4 F8 N5 P2 Rh'
_chemical_formula_weight         1173.25
_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                 98.1470(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.71475(7)
_cell_length_b                   23.1930(2)
_cell_length_c                   19.8589(2)
_cell_measurement_reflns_used    22518
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2520
_cell_measurement_theta_min      3.8086
_cell_volume                     5341.21(8)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31348
_diffrn_reflns_theta_full        76.45
_diffrn_reflns_theta_max         76.45
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    5.558
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
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    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.1405
_exptl_crystal_size_mid          0.1347
_exptl_crystal_size_min          0.0968
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         9487
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0291P)^2^+4.2922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0552
_reflns_number_gt                9385
_reflns_number_total             9487
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om5b00809_si_002.cif
_cod_data_source_block           alb143az_7
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4088023