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_4348955
_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 H33 N3 Pt'
_chemical_formula_sum            'C34 H33 N3 Pt'
_chemical_formula_weight         678.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                106.698(5)
_cell_angle_beta                 104.862(5)
_cell_angle_gamma                91.891(5)
_cell_formula_units_Z            2
_cell_length_a                   8.062(4)
_cell_length_b                   13.212(6)
_cell_length_c                   15.156(7)
_cell_measurement_reflns_used    6260
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.49
_cell_volume                     1484.6(12)
_computing_cell_refinement       'Apex2 v2013.2-0 (Bruker AXS, 2008)'
_computing_data_collection       'Apex2 v2013.2-0 (Bruker AXS, 2008)'
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_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 0.997
_diffrn_measured_fraction_theta_max 0.986
_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
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_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17732
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.022
_diffrn_reflns_theta_min         1.819
_exptl_absorpt_coefficient_mu    4.752
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.11
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_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.351
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6116
_reflns_number_total             7079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00102a2.cif
_cod_data_source_block           NNN_Pt_sidearm
_cod_database_code               4348955
_computing_refinement_gui        'shelXle rev 647 (Hubschle et al, 2011)'
_shelxl_version_number           2013-4
_shelx_res_checksum              21181
_shelx_hkl_checksum              97118
_shelx_fab_checksum              40672