Modulating the σ-Accepting Properties of an Antimony Z-type Ligand via Anion Abstraction: Remote-Controlled Reactivity of the Coordinated Platinum Atom.
You, Di; Yang, Haifeng; Sen, Srobona; Gabbaï, François P; Journal of the American Chemical Society 140 (2018) 9644–9651; doi:10.1021/jacs.8b05520

data_4132688
_publ_section_title
;
 Modulating the \s-Accepting Properties of an Antimony Z-type Ligand via
 Anion Abstraction: Remote-Controlled Reactivity of the Coordinated
 Platinum Atom.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9644
_journal_page_last               9651
_journal_paper_doi               10.1021/jacs.8b05520
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'C86 H78 F4 N2 P4 Pt2 Sb2, 2(B C18 F16), 3.14(C H2 Cl2)'
_chemical_formula_sum            'C125.14 H84.28 B2 Cl6.28 F36 N2 P4 Pt2 Sb2'
_chemical_formula_weight         3301.71
_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
_audit_creation_date             2016-09-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                115.125(3)
_cell_angle_beta                 102.188(3)
_cell_angle_gamma                92.038(3)
_cell_formula_units_Z            1
_cell_length_a                   8.936(2)
_cell_length_b                   19.412(5)
_cell_length_c                   20.369(5)
_cell_measurement_reflns_used    8681
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      24.558
_cell_measurement_theta_min      2.281
_cell_volume                     3095.5(13)
_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      110.0
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28678
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.407
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         1.963
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.977
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0900 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.8481.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.503
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.819
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         10184
_refine_ls_number_restraints     309
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0421P)^2^+8.5420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8685
_reflns_number_total             10184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05520_si_002.cif
_cod_data_source_block           6
_cod_original_cell_volume        3095.3(13)
_cod_database_code               4132688
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.316
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim N1A \\sim
C38A \\sim C39A \\sim C40A \\sim C41A \\sim C42A \\sim C43A: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N1) = Uanis(N1A)
3. Rigid body (RIGU) restrains
 N1, C38, C39, C40, C41, C42, C43, N1A, C38A, C39A, C40A, C41A, C42A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{N1, C38, C39, C40, C41, C42, C43} sigma for 1-2: 0.005, 1-3: 0.04
as
{N1A, C38A, C39A, C40A, C41A, C42A, C43A}
5. Others
 Sof(N1A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=
 Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=Sof(H42C)=
 Sof(H42D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=1-FVAR(1)
 Sof(N1)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=
 Sof(H43A)=Sof(H43B)=FVAR(1)
 Fixed Sof: Cl3S(0.57) Cl4S(0.57) C2S(0.57) H2SA(0.57) H2SB(0.57)
6.a Ternary CH refined with riding coordinates:
 C38(H38), C38A(H38A)
6.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C39A(H39C,H39D), C40A(H40C,H40D), C41A(H41C,H41D), C42A(H42C,H42D),
 C43A(H43C,H43D), C1S(H1SA,H1SB), C2S(H2SA,H2SB)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              10778
_shelx_hkl_checksum              86231
_shelx_fab_checksum              68064
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'