Diaminocarbene and Phosphonium Ylide Ligands: A Systematic Comparison of their Donor Character
Yves Canac; Christine Lepetit; Mohammed Abdalilah; Carine Duhayon; Remi Chauvin; Journal of the American Chemical Society 130 (2008) 8406–8413; doi:10.1021/ja801159v

data_4107948
_publ_contact_author_address
; 
Laboratoire de Chimie de Coordination
205 route de Narbonne
31077 Toulouse Cedex 04, FRANCE
;
_publ_contact_author_email       yves.canac@lcc-toulouse.fr
_publ_contact_author_name        'Yves Canac'
_publ_section_title
;
 Diaminocarbene and Phosphonium Ylide Ligands: A Systematic Comparison of
 their Donor Character
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8406
_journal_page_last               8413
_journal_paper_doi               10.1021/ja801159v
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C16 H14 N4 O2 Rh, C F3 O3 S, 2(C H2 Cl2)'
_chemical_formula_sum            'C19 H18 Cl4 F3 N4 O5 Rh S'
_chemical_formula_weight         716.15
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-11-23
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5516(5)
_cell_length_b                   11.7085(4)
_cell_length_c                   16.9923(6)
_cell_measurement_reflns_used    7562
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     2696.15(17)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_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  0.072
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28592
_diffrn_reflns_theta_full        30.974
_diffrn_reflns_theta_max         32.264
_diffrn_reflns_theta_min         2.830
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       planar
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         1803
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.001235
_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: 
 0.405 -0.158E-01 0.188 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0640
_refine_ls_wR_factor_gt          0.0302
_refine_ls_wR_factor_ref         0.0302
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                1803
_reflns_number_total             3723
_reflns_threshold_expression     I>1.7\s(I)
_cod_data_source_file            ja801159v-file001.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P n m a '
_cod_original_formula_sum        'C19 H18 Cl4 F3 N4 O5 Rh1 S1'
_cod_database_code               4107948