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_4331600
_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         'C38 H34 N4 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C40 H34 F6 N4 O6 P2 S2'
_chemical_formula_weight         906.80
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 116.15(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.633(3)
_cell_length_b                   22.942(5)
_cell_length_c                   14.911(3)
_cell_measurement_reflns_used    8604
_cell_measurement_temperature    180
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     4800(2)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.951
_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  0.0659
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22578
_diffrn_reflns_theta_full        26.274
_diffrn_reflns_theta_max         31.279
_diffrn_reflns_theta_min         1.701
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0681
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4905
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.1191
_refine_ls_shift/su_max          0.000312
_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: 
 1.60 0.707 0.896 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1220
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1073
_reflns_limit_h_max              20
_reflns_limit_h_min              -22
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                5425
_reflns_number_total             7462
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.1134
_oxford_reflns_number_all        7434
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic3006508_si_002_2.cif
_cod_data_source_block           cpd3
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4331600