Toward new organometallic architectures: synthesis of carbene-centered rhodium and palladium bisphosphine complexes. stability and reactivity of [PC(BIm)PRh(L)][PF6] pincers.
Plikhta, Andriy; Pöthig, Alexander; Herdtweck, Eberhardt; Rieger, Bernhard; Inorganic chemistry 54 (2015) 9517–9528; doi:10.1021/acs.inorgchem.5b01428

data_4346419
_publ_section_title
;
 Toward new organometallic architectures: synthesis of carbene-centered
 rhodium and palladium bisphosphine complexes. stability and reactivity of
 [PC(BIm)PRh(L)][PF6] pincers.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9517
_journal_page_last               9528
_journal_paper_doi               10.1021/acs.inorgchem.5b01428
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C66 H57 N4 P4 Rh2, F6 P, C4 H10 O'
_chemical_formula_sum            'C70 H67 F6 N4 O P5 Rh2'
_chemical_formula_weight         1454.92
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                99.852(2)
_cell_angle_beta                 103.228(1)
_cell_angle_gamma                94.338(1)
_cell_formula_units_Z            2
_cell_length_a                   12.0213(3)
_cell_length_b                   15.1548(4)
_cell_length_c                   18.3327(5)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.4526
_cell_measurement_theta_min      2.3267
_cell_volume                     3180.27(15)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'MONTEL optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            82566
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         12981
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0246P)^2^+2.2600P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                11336
_reflns_number_total             12981
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic5b01428_si_002.cif
_cod_data_source_block           plian3_0m
_cod_database_code               4346419
_shelxl_version_number           2014-1
_shelx_res_checksum              98867
_shelx_hkl_checksum              96396