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_1531941
_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, C F3 O3 S, 2(C4 H10 O)'
_chemical_formula_sum            'C71 H94 F3 N2 O5 Pt S Tl'
_chemical_formula_weight         1544.00
_chemical_name_common            '[TlPt(CNArDipp2)2]OTf'
_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                66.887(3)
_cell_angle_beta                 70.018(3)
_cell_angle_gamma                71.465(3)
_cell_formula_units_Z            2
_cell_length_a                   13.9500(8)
_cell_length_b                   16.2777(10)
_cell_length_c                   17.6213(10)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.33
_cell_volume                     3379.6(4)
_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      100.0
_diffrn_detector                 'Bruker Photon-100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker Photon100 Imus'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            69661
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mus'
_exptl_absorpt_coefficient_mu    4.537
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0940 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.6771.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.055
_refine_diff_density_max         2.795
_refine_diff_density_min         -2.750
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         12410
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0273P)^2^+11.3561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10267
_reflns_number_total             12410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03104d2.cif
_cod_data_source_block           JFig671
_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               1531941
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.459
_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. Rigid body (RIGU) restrains
 F1, F3, F2, C63, S1, O3, O1, O2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C30(H30), C15(H15), C18(H18), C27(H27), C54(H54), C57(H57), C45(H45), C60(H60)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C11(H11), C7(H7), C6(H6), C5(H5), C23(H23), C24(H24),
 C25(H25), C37(H37), C36(H36), C35(H35), C50(H50), C51(H51), C52(H52), C41(H41),
  C42(H42), C43(H43)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C19(H19A,H19B,
 H19C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              52297
_shelx_fab_checksum              24963
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'