Fluxionality of [(Ph3P)3M(X)] (M = Rh, Ir). The Red and Orange Forms of [(Ph3P)3Ir(Cl)]. Which Phosphine Dissociates Faster from Wilkinson's Catalyst?
Jenni Goodman; Vladimir V. Grushin; Roman B. Larichev; Stuart A. Macgregor; William J. Marshall; D. Christopher Roe; Journal of the American Chemical Society 132 (2010) 12013–12026; doi:10.1021/ja1039693

data_4102955
_publ_section_title
;
 Fluxionality of [(Ph3P)3M(X)] (M = Rh, Ir). The Red and Orange Forms of
 [(Ph3P)3Ir(Cl)]. Which Phosphine Dissociates Faster from Wilkinson's
 Catalyst?
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12013
_journal_page_last               12026
_journal_paper_doi               10.1021/ja1039693
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C54 H45 Cl Ir P3'
_chemical_formula_weight         1014.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.358(3)
_cell_length_b                   12.646(2)
_cell_length_c                   18.038(3)
_cell_measurement_reflns_used    2718
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.28
_cell_measurement_theta_min      2.23
_cell_volume                     4415.7(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1186
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39468
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    3.230
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                5940
_reflns_number_total             8987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1039693_si_002_1.cif
_cod_data_source_block           09066
_cod_original_cell_volume        4415.7(13)
_cod_database_code               4102955