Heteroligated PtII Weak-Link Approach complexes using hemilabile N-heterocyclic carbene‒thioether and phosphino‒thioether ligands
Rosen, Mari S.; Stern, Charlotte L.; Mirkin, Chad A.; Chemical Science 4 (2013) 4193–; doi:10.1039/c3sc51557e

data_1514731
_publ_section_title
;
 Heteroligated PtII Weak-Link Approach complexes using hemilabile
 N-heterocyclic carbene--thioether and phosphino--thioether ligands
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              4193
_journal_paper_doi               10.1039/c3sc51557e
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C35 H33 N2 P Pt S2, 2(B F4)'
_chemical_formula_sum            'C35 H33 B2 F8 N2 P Pt S2'
_chemical_formula_weight         945.43
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2012-09-19
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2950(3)
_cell_length_b                   9.8283(3)
_cell_length_c                   34.0318(11)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.23
_cell_volume                     3431.99(18)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.95
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            36515
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.036
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.331
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1692 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.4280.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.118
_refine_diff_density_max         2.637
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         10001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0380
_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^)+14.3517P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9644
_reflns_number_total             10001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3sc51557e.txt
_cod_data_source_block           Closed_Tweezer_Complex_7
_cod_database_code               1514731
_diffrn_reflns_sigmai/neti       0.0368
_shelx_estimated_absorpt_t_max   0.629
_shelx_estimated_absorpt_t_min   0.346
_shelx_hkl_checksum              12137
_shelx_res_checksum              71517
_shelxl_version_number           2012-4