Diphosphines with Strongly Polarized P-P Bonds: Hybrids between Covalent Molecules and Donor-Acceptor Adducts with Flexible Molecular Structures
Sebastian Burck; Kathrin Götz; Martin Kaupp; Martin Nieger; Johannes Weber; Jörn Schmedt auf der Günne; Dietrich Gudat; Journal of the American Chemical Society 131 (2009) 10763–10774; doi:10.1021/ja903156p

data_4104757
_publ_contact_author
;
        Martin Nieger
        Laboratory of Inorganic Chemistry
        Department of Chemistry
        Universitity of Helsinki
        P.O. Box 55
        FIN-00014 University of Helsinki
        Finland
;
_publ_contact_author_email       martin.nieger@helsinki.fi
_publ_contact_author_fax         '++358 9 191 50198'
_publ_contact_author_phone       '++358 9 191 50223'
_publ_section_title
;
 Diphosphines with Strongly Polarized P-P Bonds: Hybrids between Covalent
 Molecules and Donor-Acceptor Adducts with Flexible Molecular Structures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10763
_journal_page_last               10774
_journal_paper_doi               10.1021/ja903156p
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C40 H60 N2 P2'
_chemical_formula_sum            'C40 H60 N2 P2'
_chemical_formula_weight         630.84
_chemical_name_systematic
; 
 1,3-(Bis-2,6-diisopropylphenyl)-2-(2',3',4',5'-tetraethylphospholyl)-
 4,5-dimethyl-dihydro-1,3,2-diazaphosphole
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.629(2)
_cell_angle_beta                 95.211(2)
_cell_angle_gamma                104.049(2)
_cell_formula_units_Z            4
_cell_length_a                   10.6195(3)
_cell_length_b                   19.4211(6)
_cell_length_c                   20.5732(8)
_cell_measurement_reflns_used    11691
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     3834.5(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 deg.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.1689
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33389
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plates
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.849
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         13516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.849
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                6305
_reflns_number_total             13516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903156p_si_002_5.cif
_cod_data_source_block           gudat140_compound_4f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4104757