Flexible Diphosphine Ligands with Overall Charges of 0, +1, and +2: Critical Role of the Electrostatics in Favoring Trans over Cis Coordination
Yves Canac; Nathalie Debono; Christine Lepetit; Carine Duhayon; Remi Chauvin; Inorganic Chemistry 50 (2011) 10810–10819; doi:10.1021/ic201342z

data_4326654
_publ_contact_author_address
; 
Centre National de Recherche Scientifique
Laboratoire de Chimie de Coordination
205, route de Narbonne
31077 - Toulouse cedex 04
;
_publ_contact_author_email       canac@lcc-toulouse.fr
_publ_contact_author_name        'Yves Canac'
_publ_section_title
;
 Flexible Diphosphine Ligands with Overall Charges of 0, +1, and +2:
 Critical Role of the Electrostatics in Favoring Trans over Cis
 Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10810
_journal_page_last               10819
_journal_paper_doi               10.1021/ic201342z
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'C38 H34 Cl2 N4 P2 Pd, 2(C F3 O3 S), 2(C2 H3 N) '
_chemical_formula_sum            'C44 H40 Cl2 F6 N6 O6 P2 Pd S2'
_chemical_formula_weight         1166.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-01-18
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 103.697(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8049(4)
_cell_length_b                   16.7864(4)
_cell_length_c                   17.5998(5)
_cell_measurement_reflns_used    6523
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     4823.6(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.060
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45594
_diffrn_reflns_theta_full        29.106
_diffrn_reflns_theta_max         29.106
_diffrn_reflns_theta_min         2.674
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       stick
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         6390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001875
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./2F 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1283
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0330
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                6390
_reflns_number_total             12882
_reflns_threshold_expression     I>1.6\s(I)
_cod_data_source_file            ic201342z_si_002_3.cif
_cod_data_source_block           CRYSTALS_cif-cpd6
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C44 H40 Cl2 F6 N6 O6 P2 Pd1 S2'
_cod_database_code               4326654