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_4089619
_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            'C40.5 H41.5 Cl1.5 F1.5 N2.5 O4 P2 Pt'
_chemical_formula_weight         965.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.310(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.969(3)
_cell_length_b                   27.047(7)
_cell_length_c                   14.116(3)
_cell_measurement_reflns_used    9727
_cell_measurement_temperature    110
_cell_measurement_theta_max      35.43
_cell_measurement_theta_min      2.54
_cell_volume                     3803.0(17)
_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 0.997
_diffrn_measured_fraction_theta_max 0.965
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            169710
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.725
_diffrn_reflns_theta_min         2.962
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.932
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.5896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       plate
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.077
_refine_diff_density_max         2.520
_refine_diff_density_min         -2.150
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.305(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         40726
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.970
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                35172
_reflns_number_total             40726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400780q_si_001.cif
_cod_data_source_block           9
_cod_original_cell_volume        3802.8(16)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C40.50 H41.50 Cl1.50 F1.50 N2.50 O4 P2 Pt'
_cod_database_code               4089619
_shelx_estimated_absorpt_t_min   0.412
_shelx_estimated_absorpt_t_max   0.752
_shelxl_version_number           2013-3
_shelx_res_checksum              82927
_shelx_hkl_checksum              39189