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_4348954
_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         'C34 H36 N3 O Pt, C F3 O3 S, C6 H6'
_chemical_formula_sum            'C41 H42 F3 N3 O4 Pt S'
_chemical_formula_weight         924.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-06-17 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.622(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.800(7)
_cell_length_b                   19.274(10)
_cell_length_c                   15.618(8)
_cell_measurement_reflns_used    2252
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.04
_cell_measurement_theta_min      2.21
_cell_volume                     3819(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 1.000
_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  0.1470
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39393
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.922
_exptl_absorpt_coefficient_mu    3.789
_exptl_absorpt_correction_T_max  0.7335
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.622
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.00219(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7508
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4654
_reflns_number_total             7508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00102a2.cif
_cod_data_source_block           NNN_Pt_OH2_OTf
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348954
_shelx_estimated_absorpt_t_min   0.600
_shelx_estimated_absorpt_t_max   0.863
_computing_refinement_gui        'shelXle rev 647 (Hubschle et al, 2011)'
_shelxl_version_number           2013-4
_shelx_res_checksum              42821
_shelx_hkl_checksum              71113