Electrochemical and Chemical Oxidation of [Pt2(μ-pyrophosphite)4]4-Revisited: Characterization of a Nitrosyl Derivative, [Pt2(μ-pyrophosphite)4(NO)]3-
Martin A. Bennett; Suresh K. Bhargava; Alan M. Bond; Vipul Bansal; Craig M. Forsyth; Si-Xuan Guo; Steven H. Privér; Inorganic Chemistry 48 (2009) 2593–2604; doi:10.1021/ic802213v

data_4301734
_publ_section_title
;
Electrochemical and Chemical Oxidation of
[Pt2(\m-pyrophosphite)4]4-Revisited: Characterization of a Nitrosyl
Derivative, [Pt2(\m-pyrophosphite)4(NO)]3-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2593
_journal_page_last               2604
_journal_paper_doi               10.1021/ic802213v
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'3(C36 H30 N P2), H8 N O21 P8 Pt2, 2(C4 H10 O), C H2 Cl2'
_chemical_formula_sum            'C117 H120 Cl2 N4 O23 P14 Pt2'
_chemical_formula_weight         2844.83
_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                90.581(1)
_cell_angle_beta                 94.069(1)
_cell_angle_gamma                92.801(1)
_cell_formula_units_Z            2
_cell_length_a                   14.4911(4)
_cell_length_b                   16.5138(4)
_cell_length_c                   24.8553(7)
_cell_measurement_temperature    123(2)
_cell_volume                     5925.3(3)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker X8 Apex CCD'
_diffrn_measurement_method       'thin slice phi and omega scans'
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            74533
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.665
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2000)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.855
_refine_diff_density_min         -3.339
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         20508
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0824
_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^)+(0.0000P)^2^+150.6764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                14936
_reflns_number_total             20508
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802213v_si_001.cif
_cod_data_source_block           a38_07ab
_cod_database_code               4301734