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_4327100
_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_sum            'C36 H30 Cl P2 Rh'
_chemical_formula_weight         662.90
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.091(2)
_cell_angle_beta                 83.067(2)
_cell_angle_gamma                79.384(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7226(2)
_cell_length_b                   12.6361(3)
_cell_length_c                   13.7002(4)
_cell_measurement_reflns_used    22115
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.0286
_cell_measurement_theta_min      3.5885
_cell_volume                     1638.78(7)
_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 16.1978
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35493
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87497
_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    1.343
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
Some residual electron density were difficult to modelize and therefore, the
SQUEEZE function of PLATON (Spek, 2003) was used to eliminate the contribution
of the electron density in the solvent region from the intensity data, and the
solvent-free model was employed for the final refinement.
There is one cavity of 238 \%A^3^ per unitl cell. PLATON estimated that
the cavity contains 35 electrons which may correspond to a solvent molecule
of dichloromethane as suggested by chemical analyses.
;
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0608P)^2^+0.1068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                6159
_reflns_number_total             7439
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201508m_si_002_2.cif
_cod_data_source_block           AUB1
_cod_database_code               4327100