Coordination and Organometallic Chemistry of Relevance to the Rhodium-Based Catalyst for Ethylene Hydroamination
Aurélien Béthegnies; Vladislava A. Kirkina; Oleg A. Filippov; Jean-Claude Daran; Natalia V. Belkova; Elena Shubina; Rinaldo Poli; Inorganic Chemistry 50 (2011) 12539–12552; doi:10.1021/ic201508m

data_4327099
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France
;
_publ_contact_author_email       ' daran@lcc-toulouse.fr '
_publ_contact_author_fax         ' (33) 5 61 55 30 03 '
_publ_contact_author_name        'Daran, Jean-Claude'
_publ_contact_author_phone       ' (33) 5 61 33 31 18 '
_publ_section_title
;
 Coordination and Organometallic Chemistry of Relevance to the
 Rhodium-Based Catalyst for Ethylene Hydroamination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12539
_journal_page_last               12552
_journal_paper_doi               10.1021/ic201508m
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C54 H45 I P3 Rh'
_chemical_formula_sum            'C54 H45 I P3 Rh'
_chemical_formula_weight         1016.62
_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                   19.7950(8)
_cell_length_b                   12.6130(6)
_cell_length_c                   17.7058(8)
_cell_measurement_reflns_used    16186
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.99
_cell_volume                     4420.7(3)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2010)'
_computing_data_reduction        CrysAlisPro
_computing_publication_material  SHELXL-97
_computing_structure_refinement
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_measurement_method       '\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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24208
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro (Agilent Technologies, 2010)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       box
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
'Refinement of the Flack's parameter (Flack, 1983) based on Friedel's pairs'
_refine_ls_abs_structure_Flack   0.008(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8931
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.6448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                8194
_reflns_number_total             8931
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201508m_si_002_1.cif
_cod_data_source_block           AUB2
_cod_database_code               4327099