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_1531938
_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 Pd Tl, C32 H12 B F24, 2(C7 H8)'
_chemical_formula_sum            'C108 H102 B F24 N2 Pd Tl'
_chemical_formula_weight         2205.49
_chemical_name_common            '[(eta6-Tol)2TlPd(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             2015-07-14
_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                105.5970(10)
_cell_angle_beta                 102.3250(10)
_cell_angle_gamma                97.3080(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5519(5)
_cell_length_b                   20.2591(8)
_cell_length_c                   21.6470(8)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.45
_cell_volume                     5079.1(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 APEX Mo'
_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  0.0311
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69535
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.549
_diffrn_reflns_theta_min         1.815
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_exptl_absorpt_coefficient_mu    1.853
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction.'
_exptl_crystal_colour            Orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       Block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.848
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.069
_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     1339
_refine_ls_number_reflns         18800
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0294
_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^+6.2943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16668
_reflns_number_total             18800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03104d2.cif
_cod_data_source_block           JFig260
_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               1531938
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.700
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C74A) = Uanis(C75)
Uanis(C72A) = Uanis(C72)
Uanis(C75A) = Uanis(C70)
Uanis(C74) = Uanis(C73A)
3. Rigid body (RIGU) restrains
 C99, F24B, F1A, F24, F23B, F22, F22B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F21A, C100, F19A, F19, F20A, F20, F21
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C70, C76, C72, C71, C73, C74, C75, C75A, C72A, C76A, C71A, C73A, C70A, C74A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(F22)=1-FVAR(1)
 Sof(F22B)=FVAR(1)
 Sof(F24)=1-FVAR(2)
 Sof(F23B)=FVAR(2)
 Sof(F24B)=1-FVAR(3)
 Sof(F1A)=FVAR(3)
 Sof(F20A)=Sof(F19A)=Sof(F21A)=1-FVAR(4)
 Sof(F21)=Sof(F19)=Sof(F20)=FVAR(4)
 Sof(C72A)=Sof(C76A)=Sof(H76D)=Sof(H76E)=Sof(H76F)=Sof(C71A)=Sof(H71A)=
 Sof(C73A)=Sof(H73A)=Sof(C74A)=Sof(H74A)=Sof(C75A)=Sof(H75A)=Sof(C70A)=
 Sof(H70A)=1-FVAR(5)
 Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C74)=Sof(H74)=Sof(C75)=Sof(H75)=
 Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(C73)=Sof(H73)=FVAR(5)
5.a Ternary CH refined with riding coordinates:
 C57(H57), C48(H48), C60(H60), C27(H27), C24(H24), C15(H15), C30(H30), C45(H45)
5.b Aromatic/amide H refined with riding coordinates:
 C74(H74), C75(H75), C70(H70), C71(H71), C73(H73), C64(H64), C63(H63),
 C67(H67), C68(H68), C65(H65), C54(H54), C53(H53), C55(H55), C41(H41), C42(H42),
  C21(H21), C22(H22), C43(H43), C20(H20), C104(H104), C13(H13), C12(H12),
 C36(H36), C102(H102), C11(H11), C80(H80), C96(H96), C6(H6), C94(H94), C88(H88),
  C86(H86), C5(H5), C37(H37), C35(H35), C82(H82), C7(H7), C90(H90), C106(H106),
 C78(H78), C98(H98), C71A(H71A), C73A(H73A), C74A(H74A), C75A(H75A), C70A(H70A)
5.c Fitted hexagon refined as free rotating group:
 C74(C75,C70,C71,C72,C73)
5.d Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C49(H49A,H49B,H49C), C69(H69A,H69B,H69C), C50(H50A,H50B,
 H50C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C17(H17A,H17B,H17C), C46(H46A,
 H46B,H46C), C25(H25A,H25B,H25C), C16(H16A,H16B,H16C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C29(H29A,H29B,H29C), C47(H47A,H47B,H47C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C26(H26A,H26B,H26C),
 C76A(H76D,H76E,H76F)
;
_shelx_res_checksum              96460
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'