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_1531946
_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         'C62 H74 N2 Pt Tl, C32 H12 B F24'
_chemical_formula_sum            'C94 H86 B F24 N2 Pt Tl'
_chemical_formula_weight         2109.91
_chemical_name_common            '[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             2015-07-20
_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                76.597(2)
_cell_angle_beta                 79.378(3)
_cell_angle_gamma                89.566(3)
_cell_formula_units_Z            4
_cell_length_a                   14.6265(7)
_cell_length_b                   20.6542(10)
_cell_length_c                   31.1986(15)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.183
_cell_measurement_theta_min      2.208
_cell_volume                     9005.2(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (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, 2008)'
_computing_structure_solution    'ShelXT (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 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.1177
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            103583
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_min         1.453
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_exptl_absorpt_coefficient_mu    3.434
_exptl_absorpt_correction_T_max  0.0439
_exptl_absorpt_correction_T_min  0.0238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0865 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.5421.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       Block
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.051
_refine_diff_density_max         2.130
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2461
_refine_ls_number_reflns         32879
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0454P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18967
_reflns_number_total             32879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03104d2.cif
_cod_data_source_block           JFig1197
_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_database_code               1531946
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.710
_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. Uiso/Uaniso restraints and constraints
Uanis(C82) = Uanis(C82A)
Uanis(C81A) = Uanis(C81)
3. Rigid body (RIGU) restrains
 C82, C82A, C81, C80
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F10A, F10, C147, C1A, F11A, F11, C145, F12A, F12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F30, F30A, C179, F31A, F31, F32A, F32
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F20A, F20, C155, F21A, F21, F19A, F19
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F16, F16A, C140, F17, F17A, F18, F18A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F24, F24A, C156, F22A, F22, F23A, F23
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F45, F45A, C163, F46A, F46, F47A, F47
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F38, F37A, F37, F38A, C172, F36A, F36
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(H80A)=Sof(C82A)=Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C81A)=Sof(H81D)=
 Sof(H81E)=Sof(H81F)=1-FVAR(1)
 Sof(H80)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=Sof(H82A)=Sof(H82B)=
 Sof(H82C)=FVAR(1)
 Sof(F12A)=Sof(F10A)=Sof(F11A)=Sof(C1A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=Sof(C147)=FVAR(2)
 Sof(F30A)=Sof(F31A)=Sof(F32A)=1-FVAR(3)
 Sof(F32)=Sof(F31)=Sof(F30)=FVAR(3)
 Sof(F46A)=Sof(F45A)=Sof(F47A)=1-FVAR(4)
 Sof(F47)=Sof(F45)=Sof(F46)=FVAR(4)
 Sof(F17A)=Sof(F18A)=Sof(F16A)=1-FVAR(5)
 Sof(F18)=Sof(F16)=Sof(F17)=FVAR(5)
 Sof(F21A)=Sof(F20A)=Sof(F19A)=1-FVAR(6)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(6)
 Sof(F38A)=Sof(F36A)=Sof(F37A)=1-FVAR(7)
 Sof(F38)=Sof(F36)=Sof(F37)=FVAR(7)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(8)
 Sof(F22)=Sof(F24)=Sof(F23)=FVAR(8)
5.a Ternary CH refined with riding coordinates:
 C89(H89), C110(H110), C20(H20), C107(H107), C50(H50), C119(H119), C17(H17),
 C77(H77), C47(H47), C122(H122), C32(H32), C92(H92), C80(H80), C80(H80A),
 C29(H29), C59(H59), C62(H62)
5.b Aromatic/amide H refined with riding coordinates:
 C170(H170), C174(H174), C166(H166), C186(H186), C182(H182), C98(H98),
 C168(H168), C160(H160), C184(H184), C67(H67), C97(H97), C158(H158), C142(H142),
  C117(H117), C178(H178), C25(H25), C146(H146), C69(H69), C68(H68), C134(H134),
 C144(H144), C9(H9), C45(H45), C116(H116), C176(H176), C162(H162), C128(H128),
 C85(H85), C104(H104), C130(H130), C126(H126), C39(H39), C86(H86), C8(H8),
 C13(H13), C37(H37), C150(H150), C138(H138), C7(H7), C103(H103), C87(H87),
 C99(H99), C154(H154), C115(H115), C44(H44), C43(H43), C38(H38), C152(H152),
 C14(H14), C105(H105), C26(H26), C136(H136), C73(H73), C75(H75), C15(H15),
 C57(H57), C55(H55), C27(H27), C56(H56), C74(H74)
5.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C18(H18A,H18B,H18C), C111(H11A,H11B,
 H11C), C30(H30A,H30B,H30C), C109(H10A,H10B,H10C), C91(H91A,H91B,H91C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C112(H11D,H11E,H11F), C90(H90A,H90B,
 H90C), C22(H22A,H22B,H22C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C),
 C120(H12A,H12B,H12C), C49(H49A,H49B,H49C), C108(H10D,H10E,H10F), C121(H12D,
 H12E,H12F), C33(H33A,H33B,H33C), C79(H79A,H79B,H79C), C31(H31A,H31B,H31C),
 C61(H61A,H61B,H61C), C78(H78A,H78B,H78C), C34(H34A,H34B,H34C), C48(H48A,H48B,
 H48C), C124(H12G,H12H,H12I), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C),
 C123(H12J,H12K,H12L), C81(H81A,H81B,H81C), C64(H64A,H64B,H64C), C82(H82A,H82B,
 H82C), C82A(H82D,H82E,H82F), C81A(H81D,H81E,H81F)
;
_shelx_res_checksum              92071
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'