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_4316020
_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 N3 P4, C D Cl3'
_chemical_formula_sum            'C64 H51 Cl3 D N3 P4'
_chemical_formula_weight         1094.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   34.4488(5)
_cell_length_b                   34.4488(5)
_cell_length_c                   27.7148(6)
_cell_measurement_reflns_used    26924
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.55
_cell_volume                     28483.3(8)
_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    'SHELXS-97 (Sheldrick., 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            76812
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10224
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
;
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     745
_refine_ls_number_reflns         11141
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+41.0566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                8252
_reflns_number_total             11141
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100221w_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C64 H51 D Cl3 N3 P4'
_cod_database_code               4316020