Metal-only Lewis pairs between group 10 metals and Tl(i) or Ag(i): insights into the electronic consequences of Z-type ligand binding
Barnett, Brandon R.; Moore, Curtis E.; Chandrasekaran, Perumalreddy; Sproules, Stephen; Rheingold, Arnold L.; DeBeer, Serena; Figueroa, Joshua S.; Chem. Sci. 6 (2015) 7169–; doi:10.1039/C5SC03104D

data_1531945
_publ_section_title
;
 Metal-only Lewis pairs between group 10 metals and Tl(i) or Ag(i):
 insights into the electronic consequences of Z-type ligand binding
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              7169
_journal_paper_doi               10.1039/C5SC03104D
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C66 H84 N2 O Pt Tl, C32 H12 B F24'
_chemical_formula_sum            'C98 H96 B F24 N2 O Pt Tl'
_chemical_formula_weight         2184.03
_chemical_name_common            '[(Et2O)TlPt(CNArDipp2)2]BArF'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-22 deposited with the CCDC.
2015-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                99.200(4)
_cell_angle_beta                 90.224(4)
_cell_angle_gamma                90.514(4)
_cell_formula_units_Z            4
_cell_length_a                   12.7326(12)
_cell_length_b                   26.642(3)
_cell_length_c                   28.428(3)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.791
_cell_measurement_theta_min      2.208
_cell_volume                     9518.8(17)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            115702
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.474
_diffrn_reflns_theta_min         1.784
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_exptl_absorpt_coefficient_mu    3.253
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0749 before and 0.0418 after correction. The Ratio of minimum to maximum transmission is 0.7411. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       Block
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.513
_exptl_crystal_size_mid          0.507
_exptl_crystal_size_min          0.402
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2838
_refine_ls_number_reflns         35166
_refine_ls_number_restraints     706
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0268P)^2^+18.8661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28888
_reflns_number_total             35166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03104d2.cif
_cod_data_source_block           JFig814
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_colour_primary' value 'Yellow' changed to 'yellow'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1531937--1531946.cif.
;
_cod_original_cell_volume        9518.9(16)
_cod_database_code               1531945
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.355
_shelx_estimated_absorpt_t_min   0.286
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C191-C192
 1.5 with sigma of 0.01
 C196-C195
 1.5 with sigma of 0.01
 C192-C191 = C1B-C1A = C1F-C1E = C190-C189
 1.54 with sigma of 0.02
 O2-C190 = O2A-C1E = O2-C191 = O2A-C1A
 1.4 with sigma of 0.02
 C1H-C1G = C196-C195
 1.54 with sigma of 0.02
 O1-C1G = O1-C195
 1.4 with sigma of 0.02
 C49A-C47 = C49-C47 = C48-C47 = C48A-C47
 1.54 with sigma of 0.02
 C61-C59 = C61A-C59 = C60-C59 = C60A-C59
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Tl2) = Uanis(Tl2A)
Uanis(C191) = Uanis(C1A)
Uanis(C1B) = Uanis(C192)
Uanis(O2) = Uanis(O2A)
Uanis(C1C) = Uanis(C156)
Uanis(C1D) = Uanis(C172)
Uanis(Pt2A) = Uanis(Pt2)
Uanis(C190) = Uanis(C1E)
Uanis(C189) = Uanis(C1F)
Uanis(C195) = Uanis(C1G)
Uanis(C1H) = Uanis(C196)
Uanis(C60) = Uanis(C60A)
Uanis(C61A) = Uanis(C61)
Uanis(C48) = Uanis(C48A)
Uanis(C49A) = Uanis(C49)
4. Rigid body (RIGU) restrains
 F38A, F39, F39A, C147, F37, F37A, F38
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F25, F27A, C131, F27, F26A, F26, F25A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F26, F27, F25, C131, F27A, F25A, F26A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F40, F41, C148, F42, F40A, F42A, F41A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F43, F45, C156, F44, F44A, F43A, F45A, C1C
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F37, C147, F39, F39A, F37A, F38A, F38
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F10, F11, F12, C179, F12A, F10A, F11A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C167, F3, F1, F2, C172, F2A, C1D, F1A, F3A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C171, F6, F5, F4, F5A, F4A, F6A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F14, C180, F15, F13, F14A, F13A, F15A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F16, F18, F17, C188, F16A, F18A, F17A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F46, F48, C155, F46A, F48A, F47A, F47
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F21, F20, F19, C187, F19A, F20A, F21A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F6A, F6, C171, F4A, F4, F5A, F5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1B, C191, O2, O2A, C1A, C192, C1E, C190, C189, C1F
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C70, C81, C71, C72, C80, C82, C73, C76, C77, C78, C79, C78A, C77A, C79A, C76A,
  C71A, C72A, C80A, C81A, C82A, C73A, C74A, C75A, C74, C75
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C61A, C61, C59, C60, C60A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C49A, C49, C47, C48, C48A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F27A)=Sof(F25A)=Sof(F26A)=1-FVAR(1)
 Sof(F26)=Sof(F27)=Sof(F25)=FVAR(1)
 Sof(F39A)=Sof(F37A)=Sof(F38A)=1-FVAR(2)
 Sof(F37)=Sof(F38)=Sof(F39)=FVAR(2)
 Sof(Tl2A)=Sof(Pt2A)=Sof(O2A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(H1BC)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=
 Sof(H1FC)=1-FVAR(3)
 Sof(Pt2)=Sof(Tl2)=Sof(C189)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O2)=Sof(C190)=
 Sof(H19A)=Sof(H19B)=Sof(C191)=Sof(H19C)=Sof(H19D)=Sof(C192)=Sof(H19E)=
 Sof(H19F)=Sof(H19G)=FVAR(3)
 Sof(F5A)=Sof(F4A)=Sof(F6A)=1-FVAR(4)
 Sof(F6)=Sof(F5)=Sof(F4)=FVAR(4)
 Sof(F44A)=Sof(F43A)=Sof(F45A)=Sof(C1C)=1-FVAR(5)
 Sof(F43)=Sof(F45)=Sof(C156)=Sof(F44)=FVAR(5)
 Sof(F12A)=Sof(F10A)=Sof(F11A)=1-FVAR(6)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(6)
 Sof(F14A)=Sof(F13A)=Sof(F15A)=1-FVAR(7)
 Sof(F14)=Sof(F15)=Sof(F13)=FVAR(7)
 Sof(F16A)=Sof(F18A)=Sof(F17A)=1-FVAR(8)
 Sof(F16)=Sof(F18)=Sof(F17)=FVAR(8)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(9)
 Sof(F21)=Sof(F20)=Sof(F19)=FVAR(9)
 Sof(F40A)=Sof(F42A)=Sof(F41A)=1-FVAR(10)
 Sof(F40)=Sof(F41)=Sof(F42)=FVAR(10)
 Sof(F46A)=Sof(F48A)=Sof(F47A)=1-FVAR(11)
 Sof(F46)=Sof(F48)=Sof(F47)=FVAR(11)
 Sof(F2A)=Sof(C1D)=Sof(F3A)=Sof(F1A)=1-FVAR(12)
 Sof(F3)=Sof(F1)=Sof(F2)=Sof(C172)=FVAR(12)
 Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=Sof(C77A)=Sof(H77A)=Sof(C79A)=
 Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C76A)=Sof(C71A)=Sof(C72A)=Sof(C73A)=
 Sof(H73A)=Sof(C74A)=Sof(H74A)=Sof(C75A)=Sof(H75A)=Sof(C80A)=Sof(H80A)=
 Sof(C81A)=Sof(H81D)=Sof(H81E)=Sof(H81F)=Sof(C82A)=Sof(H82D)=Sof(H82E)=
 Sof(H82F)=1-FVAR(13)
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C71)=Sof(C72)=Sof(C80)=Sof(H80)=
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C73)=Sof(H73)=Sof(C74)=Sof(H74)=
 Sof(C75)=Sof(H75)=Sof(C76)=Sof(C77)=Sof(H77)=Sof(C78)=Sof(H78A)=Sof(H78B)=
 Sof(H78C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=FVAR(13)
 Sof(H92A)=Sof(C94A)=Sof(H94D)=Sof(H94E)=Sof(H94F)=Sof(C93A)=Sof(H93D)=
 Sof(H93E)=Sof(H93F)=1-FVAR(14)
 Sof(H92)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=Sof(C94)=Sof(H94A)=Sof(H94B)=
 Sof(H94C)=FVAR(14)
 Sof(C1G)=Sof(H1GA)=Sof(H1GB)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=1-FVAR(15)
 Sof(C195)=Sof(H19P)=Sof(H19Q)=Sof(C196)=Sof(H19R)=Sof(H19S)=Sof(H19T)=FVAR(15)
 Sof(H59A)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61A)=Sof(H61D)=
 Sof(H61E)=Sof(H61F)=1-FVAR(16)
 Sof(H59)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=
 Sof(H61C)=FVAR(16)
 Sof(H47A)=Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(C48A)=Sof(H48D)=
 Sof(H48E)=Sof(H48F)=1-FVAR(17)
 Sof(H47)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=FVAR(17)
6.a Ternary CH refined with riding coordinates:
 C59(H59), C59(H59A), C20(H20), C17(H17), C62(H62), C35(H35), C38(H38),
 C47(H47), C47(H47A), C50(H50), C80(H80), C77(H77), C92(H92), C92(H92A),
 C89(H89), C122(H122), C119(H119), C110(H110), C107(H107), C77A(H77A),
 C80A(H80A)
6.b Secondary CH2 refined with riding coordinates:
 C194(H19N,H19O), C195(H19P,H19Q), C190(H19A,H19B), C191(H19C,H19D), C1A(H1AA,
 H1AB), C1E(H1EA,H1EB), C1G(H1GA,H1GB)
6.c Me refined with riding coordinates:
 C1B(H1BA,H1BB,H1BC)
6.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C134(H134), C130(H130), C144(H144), C142(H142), C146(H146),
 C138(H138), C136(H136), C154(H154), C152(H152), C150(H150), C126(H126),
 C128(H128), C13(H13), C14(H14), C15(H15), C9(H9), C8(H8), C7(H7), C55(H55),
 C56(H56), C57(H57), C31(H31), C32(H32), C33(H33), C27(H27), C25(H25), C45(H45),
  C44(H44), C43(H43), C67(H67), C68(H68), C69(H69), C73(H73), C74(H74),
 C75(H75), C85(H85), C86(H86), C87(H87), C115(H115), C116(H116), C117(H117),
 C97(H97), C98(H98), C99(H99), C105(H105), C104(H104), C103(H103), C178(H178),
 C186(H186), C168(H168), C170(H170), C166(H166), C162(H162), C160(H160),
 C158(H158), C174(H174), C176(H176), C182(H182), C184(H184), C73A(H73A),
 C74A(H74A), C75A(H75A)
6.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C19(H19H,H19I,H19J), C64(H64A,H64B,
 H64C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C52(H52A,
 H52B,H52C), C51(H51A,H51B,H51C), C81(H81A,H81B,H81C), C91(H91A,H91B,H91C),
 C90(H90A,H90B,H90C), C123(H12A,H12B,H12C), C124(H12D,H12E,H12F), C121(H12G,
 H12H,H12I), C111(H11A,H11B,H11C), C109(H10A,H10B,H10C), C193(H19K,H19L,H19M),
 C189(H18A,H18B,H18C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,
 H63C), C37(H37A,H37B,H37C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C), C82(H82A,
 H82B,H82C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C93(H93A,H93B,H93C),
 C94(H94A,H94B,H94C), C120(H12J,H12K,H12L), C112(H11D,H11E,H11F), C108(H10D,
 H10E,H10F), C196(H19R,H19S,H19T), C192(H19E,H19F,H19G), C18(H18D,H18E,H18F),
 C1F(H1FA,H1FB,H1FC), C78A(H78D,H78E,H78F), C79A(H79D,H79E,H79F), C81A(H81D,
 H81E,H81F), C82A(H82D,H82E,H82F), C94A(H94D,H94E,H94F), C93A(H93D,H93E,H93F),
 C1H(H1HA,H1HB,H1HC), C60A(H60D,H60E,H60F), C61A(H61D,H61E,H61F), C49A(H49D,
 H49E,H49F), C48A(H48D,H48E,H48F)
;
_shelx_res_checksum              26114
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'