P(CH)P Pincer Rhodium(I) Complexes: The Key Role of Electron-Poor Imidazoliophosphine Extremities
Cécile Barthes; Christine Lepetit; Yves Canac; Carine Duhayon; Davit Zargarian; Remi Chauvin; Inorganic Chemistry 52 (2013) 48–58; doi:10.1021/ic3006508

data_4331602
_publ_contact_author_address
; 
LCC-CNRS ou Laboratoire de Chimie de Coordination du CNRS
205 route de Narbonne
BP 44099
31077 TOULOUSE CEDEX 4
;
_publ_contact_author_email       canac@lcc-toulouse.fr
_publ_contact_author_name        'Yves Canac'
_publ_section_title
;
 P(CH)P Pincer Rhodium(I) Complexes: The Key Role of Electron-Poor
 Imidazoliophosphine Extremities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              48
_journal_page_last               58
_journal_paper_doi               10.1021/ic3006508
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C39 H34 Cl N4 O P2 Rh, 2(C F3 O3 S)'
_chemical_formula_sum            'C41 H34 Cl F6 N4 O7 P2 Rh S2'
_chemical_formula_weight         1073.17
_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
_cell_angle_alpha                77.390(4)
_cell_angle_beta                 79.713(4)
_cell_angle_gamma                68.869(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7519(12)
_cell_length_b                   13.7106(13)
_cell_length_c                   13.8297(13)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    180
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     2187.7(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55848
_diffrn_reflns_theta_full        30.919
_diffrn_reflns_theta_max         30.919
_diffrn_reflns_theta_min         1.722
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       stick
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         11019
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002824
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.483 0.620E-01 0.149 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0395
_refine_ls_wR_factor_gt          0.0315
_refine_ls_wR_factor_ref         0.0306
_reflns_limit_h_max              18
_reflns_limit_h_min              -17
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                11583
_reflns_number_total             13792
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0299
_oxford_reflns_number_all        13756
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic3006508_si_002_3.cif
_cod_data_source_block           cpd5
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C41 H34 Cl1 F6 N4 O7 P2 Rh1 S2'
_cod_database_code               4331602