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_4335201
_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         'C74.92 H76.76 Br5.08 N4 O4 P4 Pt2'
_chemical_formula_sum            'C18.73 H19.19 Br1.27 N O P Pt0.5'
_chemical_formula_weight         504.30
_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                87.58(3)
_cell_angle_beta                 81.98(3)
_cell_angle_gamma                76.46(3)
_cell_formula_units_Z            4
_cell_length_a                   9.915(2)
_cell_length_b                   13.179(3)
_cell_length_c                   19.395(4)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     2439.7(10)
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13822
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    5.048
_exptl_absorpt_correction_T_max  0.7864
_exptl_absorpt_correction_T_min  0.2866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       needles
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_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         1.221
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                5642
_reflns_number_total             8494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400576m_si_001_6.cif
_cod_data_source_block           7
_cod_original_cell_volume        2439.7(8)
_cod_original_formula_sum        'C18.73 H19.19 Br1.27 N O P Pt0.50'
_cod_database_code               4335201