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_4089614
_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            'C38 H40 N2 O2 P2 Pt'
_chemical_formula_weight         813.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.917(8)
_cell_length_b                   13.679(5)
_cell_length_c                   27.254(8)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.40
_cell_volume                     6680(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    SIR92
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.957
_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  0.0986
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            165758
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        33.610
_diffrn_reflns_theta_max         34.927
_diffrn_reflns_theta_min         2.721
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.334
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       prism
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.852
_refine_diff_density_min         -2.231
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         13997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+15.5018P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8992
_reflns_number_total             13997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400780q_si_001.cif
_cod_data_source_block           4a
_cod_database_code               4089614
_shelx_estimated_absorpt_t_min   0.633
_shelx_estimated_absorpt_t_max   0.819
_shelxl_version_number           2012-9
_shelx_res_checksum              11882
_shelx_hkl_checksum              4498