Versatile New C3-Symmetric Tripodal Tetraphosphine Ligands; Structural Flexibility to Stabilize CuI and RhI Species and Tune Their Reactivity
Jeroen Wassenaar; Maxime A. Siegler; Anthony L. Spek; Bas de Bruin; Joost N. H. Reek; Jarl Ivar van der Vlugt; Inorganic Chemistry 49 (2010) 6495–6508; doi:10.1021/ic100221w

data_4316027
_publ_section_title
;
 Versatile New C3-Symmetric Tripodal Tetraphosphine Ligands; Structural
 Flexibility to Stabilize CuI and RhI Species and Tune Their Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6495
_journal_page_last               6508
_journal_paper_doi               10.1021/ic100221w
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C63 H51 Cl N3 P4 Rh, F6 P, 3(C H2 Cl2)'
_chemical_formula_sum            'C66 H57 Cl7 F6 N3 P5 Rh'
_chemical_formula_weight         1512.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.963(2)
_cell_angle_beta                 110.874(2)
_cell_angle_gamma                101.654(3)
_cell_formula_units_Z            2
_cell_length_a                   13.2110(6)
_cell_length_b                   15.3608(8)
_cell_length_c                   17.6791(10)
_cell_measurement_reflns_used    47377
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.70
_cell_volume                     3243.8(3)
_computing_cell_refinement       'PEAKREF (Schreurs, 2005)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF08 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            83759
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'large blocks'
_exptl_crystal_F_000             1534
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         14892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0296P)^2^+4.7366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                12836
_reflns_number_total             14892
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100221w_si_002_8.cif
_cod_data_source_block           8PF6
_cod_database_code               4316027