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_4326652
_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         'C37 H31 Cl2 N4 P2 Pd, C F3 O3 S, 3(H2 O)'
_chemical_formula_sum            'C38 H37 Cl2 F3 N4 O6 P2 Pd S'
_chemical_formula_weight         974.05
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-11-17
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 93.916(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3420(4)
_cell_length_b                   26.2671(8)
_cell_length_c                   17.4220(5)
_cell_measurement_reflns_used    6235
_cell_measurement_temperature    180
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     4265.2(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.081
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46239
_diffrn_reflns_theta_full        28.028
_diffrn_reflns_theta_max         28.028
_diffrn_reflns_theta_min         1.405
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.81
_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    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.14
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9586
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         6247
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000354
_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: 
 2.19 -0.385 1.50 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0775
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0551
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7059
_reflns_number_total             10316
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0518
_oxford_reflns_number_all        10284
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'unsorted_0m in P2(1)/c'
_cod_data_source_file            ic201342z_si_002_1.cif
_cod_data_source_block           globalcpd5
_cod_original_cell_volume        4265.1(3)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C38 H37 Cl2 F3 N4 O6 P2 Pd1 S1'
_cod_database_code               4326652