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_4326653
_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         'C36 H28 N4 P2'
_chemical_formula_sum            'C36 H28 N4 P2'
_chemical_formula_weight         578.59
_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
_audit_creation_date             08-02-07
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 94.008(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   49.677(3)
_cell_length_b                   8.5858(5)
_cell_length_c                   14.3598(9)
_cell_measurement_reflns_used    6665
_cell_measurement_temperature    180
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     6109.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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  'Bruker Apex 2'
_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  0.055
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45237
_diffrn_reflns_theta_full        24.468
_diffrn_reflns_theta_max         24.468
_diffrn_reflns_theta_min         1.644
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_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    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         3828
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000506
_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: 
 1.21 1.31 0.744 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0694
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0578
_reflns_limit_h_max              57
_reflns_limit_h_min              -57
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3828
_reflns_number_total             5014
_reflns_threshold_expression     I>0.7\s(I)
_cod_data_source_file            ic201342z_si_002_2.cif
_cod_data_source_block           CRYSTALS_cif-cpd1
_cod_original_cell_volume        6109.8(6)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4326653