Cyclometallation of the NNN pincer ligand in complexes of platinum
DeMott, Jessica C.; Dekarske, John R.; McCulloch, Billy J.; Ozerov, Oleg V.; Inorganic Chemistry Frontiers 2 (2015) 912–; doi:10.1039/C5QI00102A

data_4348953
_publ_section_title
;
 Cyclometallation of the NNN pincer ligand in complexes of platinum
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              912
_journal_paper_doi               10.1039/C5QI00102A
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety
'2(C34 H36 N3 O Pt), 2(C H F3 O3 S), 2(C F3 O3 S), C6 H5 F'
_chemical_formula_sum            'C78 H79 F13 N6 O14 Pt2 S4'
_chemical_formula_weight         2089.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-06-16 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.276(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.069(4)
_cell_length_b                   14.583(2)
_cell_length_c                   26.542(6)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.34
_cell_volume                     8857(3)
_computing_cell_refinement       'Apex2 v2013.2-0 (Bruker AXS, 2008)'
_computing_data_collection       'Apex2 v2013.2-0 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT v8.18c (Bruker AXS, 2008)'
_computing_molecular_graphics    'shelXle rev 647 (Hubschle et al, 2011)'
_computing_structure_refinement  'SHELXL-2013/4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013/4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            50853
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.434
_diffrn_reflns_theta_min         2.188
_exptl_absorpt_coefficient_mu    3.338
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10085
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0425P)^2^+26.3426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8512
_reflns_number_total             10085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00102a2.cif
_cod_data_source_block           NNN-Pt-OH2-OTf-HOTF-C6H5F
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4348953
_shelx_estimated_absorpt_t_min   0.303
_shelx_estimated_absorpt_t_max   0.652
_computing_refinement_gui        'shelXle rev 647 (Hubschle et al, 2011)'
_shelxl_version_number           2013-4
_shelx_res_checksum              74819
_shelx_hkl_checksum              58350
_shelx_fab_checksum              35537