Organoplatinum Chemistry with a Dicarboxamide‒Diphosphine Ligand: Hydrogen Bonding, Cyclometalation, and a Complex with Two Metal‒Metal Donor‒Acceptor Bonds
Nasser, Nasser; Boyle, Paul D.; Puddephatt, Richard J.; Organometallics 32 (2013) 5504–; doi:10.1021/om400780q

data_4089616
_publ_section_title
;
 Organoplatinum Chemistry with a Dicarboxamide--Diphosphine Ligand:
 Hydrogen Bonding, Cyclometalation, and a Complex with Two Metal--Metal
 Donor--Acceptor Bonds
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5504
_journal_paper_doi               10.1021/om400780q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C82 H88 Cl12 N4 O4 P4 Pt4'
_chemical_formula_weight         2523.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.009(5)
_cell_length_b                   10.033(3)
_cell_length_c                   39.550(9)
_cell_measurement_reflns_used    9619
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      3.77
_cell_volume                     8733(4)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  SHELXL-2013
_computing_structure_solution    SIR2011
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            208571
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.586
_diffrn_reflns_theta_min         3.280
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    6.879
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_description       prism
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.561
_refine_diff_density_min         -1.967
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.001(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         25900
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+15.4802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                18760
_reflns_number_total             25900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400780q_si_001.cif
_cod_data_source_block           5
_cod_database_code               4089616
_shelx_estimated_absorpt_t_min   0.513
_shelx_estimated_absorpt_t_max   0.592
_shelxl_version_number           2013-3
_shelx_res_checksum              71480
_shelx_hkl_checksum              59051