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_4335197
_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 H66 Cl4 N4 O4 P4 Pt2, C6 H6'
_chemical_formula_sum            'C19.5 H18 Cl N O P Pt0.5'
_chemical_formula_weight         446.31
_chemical_name_systematic
; 
 ? 
;
_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                89.73(3)
_cell_angle_beta                 68.07(3)
_cell_angle_gamma                86.94(3)
_cell_formula_units_Z            4
_cell_length_a                   12.102(2)
_cell_length_b                   13.432(3)
_cell_length_c                   14.707(3)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     2214.2(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15210
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    3.392
_exptl_absorpt_correction_T_max  0.5804
_exptl_absorpt_correction_T_min  0.5224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       prism
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_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         0.986
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+3.7448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                7114
_reflns_number_total             7810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400576m_si_001_2.cif
_cod_data_source_block           2b
_cod_original_cell_volume        2214.2(8)
_cod_original_formula_sum        'C19.50 H18 Cl N O P Pt0.50'
_cod_database_code               4335197