A Versatile Diphosphine Ligand: cis and trans Chelation or Bridging, with Self Association through Hydrogen Bonding
Nasser Nasser; Aneta Borecki; Paul D. Boyle; Richard J. Puddephatt; Inorganic Chemistry 52 (2013) 7051–7060; doi:10.1021/ic400576m

data_4335196
_publ_contact_author_address     'University of Western Ontario'
_publ_contact_author_email       pudd@uwo.ca
_publ_contact_author_name        Puddephatt
_publ_section_title
;
 A Versatile Diphosphine Ligand: cis and trans Chelation or Bridging, with
 Self Association through Hydrogen Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7051
_journal_page_last               7060
_journal_paper_doi               10.1021/ic400576m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C72 H68 Au2 N4 O4 P4, 2(C H Cl3), 2(Cl) '
_chemical_formula_sum            'C74 H70 Au2 Cl8 N4 O4 P4'
_chemical_formula_weight         1880.75
_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                71.11(3)
_cell_angle_beta                 85.43(3)
_cell_angle_gamma                84.12(3)
_cell_formula_units_Z            1
_cell_length_a                   10.620(2)
_cell_length_b                   13.657(3)
_cell_length_c                   15.445(3)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     2105.7(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17139
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    3.855
_exptl_absorpt_correction_T_max  0.4458
_exptl_absorpt_correction_T_min  0.2701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
Sluis, P. v. d., Spek, A. L., Acta Cryst. (1990), A46, 194-201 
implemented in a more general way as the SQUEEZE procedure in PLATON
;
_refine_diff_density_max         2.159
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+5.2741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                8647
_reflns_number_total             9566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400576m_si_001_1.cif
_cod_data_source_block           1b
_cod_original_cell_volume        2105.7(7)
_cod_database_code               4335196