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_1531937
_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 Pd Tl, C32 H12 B F24'
_chemical_formula_sum            'C98 H96 B F24 N2 O Pd Tl'
_chemical_formula_weight         2095.34
_chemical_name_systematic        '[(Et2O)TlPd(CNArDipp2]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             2015-07-13
_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                99.0980(10)
_cell_angle_beta                 90.1440(10)
_cell_angle_gamma                90.5090(10)
_cell_formula_units_Z            4
_cell_length_a                   12.7422(9)
_cell_length_b                   26.6786(18)
_cell_length_c                   28.5026(19)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.21
_cell_volume                     9566.9(11)
_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      100.0
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 APEX'
_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  0.0812
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            135836
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.447
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.8891.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       Block
_exptl_crystal_F_000             4216
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.195
_refine_diff_density_max         1.168
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2560
_refine_ls_number_reflns         32575
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21660
_reflns_number_total             32575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03104d2.cif
_cod_data_source_block           jfig226
_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 'Orange' changed to 'orange'
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               1531937
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.632
_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
 C6S-C5S
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Tl2A) = Uanis(Tl2)
Uanis(O2S) = Uanis(O2SB)
Uanis(C6SB) = Uanis(C6S)
Uanis(C5SB) = Uanis(C5S)
Uanis(C7SB) = Uanis(C7S)
Uanis(C8S) = Uanis(C8SB)
4. Rigid body (RIGU) restrains
 C155, F37C, F38A, F38B, F38C, F39A, F39B, F39C, F37A, F37B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F2AA, F0AA, F1AA, C171, F0AB, F2AB, F1AB
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F4, F5, F6, C172, F5A, F4A, F6A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F10, C188, F12, F11, F12A, F11A, F10A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F16A, F16, F18, F18A, F17, F17A, C179
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F24A, F23, F23A, C180, F22A, F22, F24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F12A, F12, C188, F11, F11A, F10A, F10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F26, F27A, C139, F25A, F27, F25, F26A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C8S, C8SB, C7SB, C7S, O2SB, O2S, C5S, C6SB, C6S, C5SB
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F26A)=Sof(F27A)=Sof(F25A)=1-FVAR(1)
 Sof(F27)=Sof(F26)=Sof(F25)=FVAR(1)
 Sof(F48B)=1-FVAR(2)
 Sof(F48A)=FVAR(2)
 Sof(F5A)=Sof(F4A)=Sof(F6A)=1-FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(3)
 Sof(F12A)=Sof(F11A)=Sof(F10A)=1-FVAR(4)
 Sof(F10)=Sof(F12)=Sof(F11)=FVAR(4)
 Sof(F0AB)=Sof(F2AB)=Sof(F1AB)=1-FVAR(5)
 Sof(F2AA)=Sof(F0AA)=Sof(F1AA)=FVAR(5)
 Sof(F16A)=Sof(F18A)=Sof(F17A)=1-FVAR(6)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(6)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(7)
 Sof(F24)=Sof(F23)=Sof(F22)=FVAR(7)
 Sof(C7SB)=Sof(H7SA)=Sof(H7SB)=Sof(C8SB)=Sof(H8SA)=Sof(H8SB)=Sof(H8SC)=
 Sof(Tl2A)=Sof(O2SB)=Sof(C6SB)=Sof(H6SD)=Sof(H6SE)=Sof(H6SF)=Sof(C5SB)=
 Sof(H5SC)=Sof(H5SD)=1-FVAR(8)
 Sof(O2S)=Sof(Tl2)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=
 Sof(H6SC)=Sof(C7S)=Sof(H7SC)=Sof(H7SD)=Sof(C8S)=Sof(H8SD)=Sof(H8SE)=Sof(H8SF)=
 FVAR(8)
 Fixed Sof: F39B(0.5) F37B(0.5) F38B(0.5) F37C(0.25) F38C(0.25) F39C(0.25)
 F37A(0.25) F38A(0.25) F39A(0.25)
6.a Ternary CH refined with riding coordinates:
 C47(H47), C29(H29), C50(H50), C59(H59), C104(H104), C32(H32), C62(H62),
 C17(H17), C20(H20), C107(H107), C95(H95), C122(H122), C110(H110), C119(H119),
 C77(H77), C80(H80)
6.b Secondary CH2 refined with riding coordinates:
 C7SB(H7SA,H7SB), C1S(H1SA,H1SB), C3S(H3SA,H3SB), C5S(H5SA,H5SB), C5SB(H5SC,
 H5SD), C7S(H7SC,H7SD)
6.c Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C22(H22A,H22B,H22C), C63(H63A,H63B,
 H63C), C52(H52A,H52B,H52C), C96(H96A,H96B,H96C), C18(H18A,H18B,H18C),
 C105(H10A,H10B,H10C), C51(H51A,H51B,H51C), C123(H12A,H12B,H12C), C108(H10D,
 H10E,H10F), C30(H30A,H30B,H30C), C61(H61A,H61B,H61C), C106(H10G,H10H,H10I),
 C21(H21A,H21B,H21C), C97(H97A,H97B,H97C), C64(H64A,H64B,H64C), C124(H12D,H12E,
 H12F), C111(H11A,H11B,H11C), C60(H60A,H60B,H60C), C112(H11D,H11E,H11F),
 C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C82(H82A,H82B,H82C), C109(H10J,H10K,
 H10L), C2S(H2SA,H2SB,H2SC), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C4S(H4SA,
 H4SB,H4SC), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C121(H12G,H12H,H12I),
 C120(H12J,H12K,H12L), C81(H81A,H81B,H81C)
6.d Aromatic/amide H refined with riding coordinates:
 C144(H144), C158(H158), C166(H166), C38(H38), C182(H182), C160(H160),
 C162(H162), C142(H142), C138(H138), C39(H39), C45(H45), C174(H174), C15(H15),
 C136(H136), C178(H178), C37(H37), C176(H176), C186(H186), C154(H154), C13(H13),
  C7(H7), C134(H134), C8(H8), C68(H68), C14(H14), C168(H168), C44(H44),
 C184(H184), C170(H170), C152(H152), C150(H150), C100(H100), C9(H9), C101(H101),
  C128(H128), C87(H87), C67(H67), C126(H126), C69(H69), C86(H86), C93(H93),
 C85(H85), C57(H57), C102(H102), C130(H130), C55(H55), C146(H146), C92(H92),
 C43(H43), C91(H91), C115(H115), C117(H117), C116(H116), C75(H75), C74(H74),
 C73(H73), C56(H56), C27(H27), C25(H25), C26(H26)
6.e Idealised Me refined as rotating group:
 C8SB(H8SA,H8SB,H8SC), C6S(H6SA,H6SB,H6SC), C6SB(H6SD,H6SE,H6SF), C8S(H8SD,
 H8SE,H8SF)
;
_shelx_res_checksum              67932
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'