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_4326656
_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         'C36 H28 Cl2 N4 P2 Pd, 2(C H Cl3)'
_chemical_formula_sum            'C38 H30 Cl8 N4 P2 Pd'
_chemical_formula_weight         994.65
_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
_cell_angle_alpha                90
_cell_angle_beta                 94.954(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7655(4)
_cell_length_b                   16.8290(5)
_cell_length_c                   18.7918(6)
_cell_measurement_reflns_used    11696
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     4022.0(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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_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  0.068
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38029
_diffrn_reflns_theta_full        29.126
_diffrn_reflns_theta_max         29.126
_diffrn_reflns_theta_min         2.654
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.78
_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    1.643
_exptl_crystal_description       cube
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1326
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.000687
_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: 
 2.03 -0.625 1.43 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0564
_refine_ls_wR_factor_gt          0.0343
_refine_ls_wR_factor_ref         0.0347
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                4738
_reflns_number_total             10770
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0298
_oxford_reflns_number_all        10784
_oxford_reflns_threshold_expression_ref I>1.9\s(I)
_cod_data_source_file            ic201342z_si_002_5.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C38 H30 Cl8 N4 P2 Pd1'
_cod_database_code               4326656