Unmasking the Catalytic Activity of a Platinum Complex with a Lewis Acidic, Non-innocent Antimony Ligand.
You, Di; Gabbaï, François P; Journal of the American Chemical Society 139 (2017) 6843–6846; doi:10.1021/jacs.7b03287

data_4126126
_publ_section_title
;
 Unmasking the Catalytic Activity of a Platinum Complex with a Lewis
 Acidic, Non-innocent Antimony Ligand.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6843
_journal_page_last               6846
_journal_paper_doi               10.1021/jacs.7b03287
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C44 H39 Cl F3 N O3 P2 Pt S Sb, C F3 O3 S'
_chemical_formula_sum            'C45 H39 Cl F6 N O6 P2 Pt S2 Sb'
_chemical_formula_weight         1282.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-09-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.051(15)
_cell_length_b                   16.451(9)
_cell_length_c                   10.734(6)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.169
_cell_measurement_theta_min      2.385
_cell_volume                     4777(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46853
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.029
_diffrn_reflns_theta_min         2.266
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.772
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0853 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.8326.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.176
_refine_diff_density_max         1.891
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         4880
_refine_ls_number_restraints     367
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+17.6370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4310
_reflns_number_total             4880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03287_si_004.cif
_cod_data_source_block           dyc_sq
_cod_database_code               4126126
_shelx_estimated_absorpt_t_max   0.557
_shelx_estimated_absorpt_t_min   0.540
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P1-C1 \\sim P1-C1A
 with sigma of 0.02
 C25-C20 \\sim C25-C24 \\sim C24-C23 \\sim C23-C22 \\sim C22-C21 \\sim C21-C20
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C1A \\sim C2A \\sim C3A
\\sim C4A \\sim C5A \\sim C6A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 2
N1 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O3) = Uanis(C26)
4. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C20, C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C1, C2, C3, C4, C5, C6} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1A, C2A, C3A, C4A, C5A, C6A}
6. Others
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(H6)=FVAR(1)
 Fixed Sof: S1(0.5) F1(0.5) F2(0.5) F3(0.5) O3(0.5) C20(0.5) H20(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) C22(0.5) H22A(0.5) H22B(0.5) C23(0.5) H23A(0.5) H23B(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) C25(0.5) H25A(0.5) H25B(0.5) C26(0.5)
7.a Ternary CH refined with riding coordinates:
 C20(H20)
7.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C2A(H2A), C3A(H3A), C4A(H4A),
 C5A(H5A), C6A(H6A), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17)
7.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
;
_shelx_res_checksum              41167
_shelx_hkl_checksum              81872
_shelx_fab_checksum              96802
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'