Isolable iodosylarene and iodoxyarene adducts of Co and their O-atom transfer and C-H activation reactivity.
Hill, Ethan A.; Kelty, Margaret L.; Filatov, Alexander S.; Anderson, John S.; Chemical science 9 (2018) 4493–4499; doi:10.1039/c8sc01167b

data_1549286
_publ_section_title
;
 Isolable iodosylarene and iodoxyarene adducts of Co and their O-atom
 transfer and C-H activation reactivity.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              4493
_journal_page_last               4499
_journal_paper_doi               10.1039/c8sc01167b
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety
'C31 H47 B Co I N6 O4 S, C32 H12 B F24, C4 H8 O, C4 H10 O'
_chemical_formula_sum            'C71 H77 B2 Co F24 I N6 O6 S'
_chemical_formula_weight         1805.89
_chemical_name_systematic        '[CoTptBuPhIO2][BArF4]'
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-23 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                69.338(4)
_cell_angle_beta                 77.588(5)
_cell_angle_gamma                78.279(5)
_cell_formula_units_Z            2
_cell_length_a                   13.018(3)
_cell_length_b                   17.299(4)
_cell_length_c                   19.933(4)
_cell_measurement_reflns_used    9444
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.150
_cell_measurement_theta_min      2.438
_cell_volume                     4062.0(16)
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'XL-2018/1 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 30
_diffrn_detector_type            'CMOS pixel array detector'
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       'phi rotation'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Si(111) & Si(311)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            114410
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         16.214
_diffrn_reflns_theta_min         0.739
_diffrn_source                   synchrotron
_diffrn_source_type
'Insertion Device, Station 15 ID-B, APS, Argonne Nat'l Lab'
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1262 before and 0.0679 after correction. 
The Ratio of minimum to maximum transmission is 0.8566. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             1830
_exptl_crystal_size_max          0.004
_exptl_crystal_size_mid          0.003
_exptl_crystal_size_min          0.003
_refine_diff_density_max         2.228
_refine_diff_density_min         -2.107
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         19783
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0624
_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^)+(0.1228P)^2^+9.8748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.1990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17696
_reflns_number_total             19783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01167b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1549282--1549287.cif.'
_cod_original_cell_volume        4062.0(14)
_cod_database_code               1549286
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.999
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F5X-C39 \\sim F4-C39 \\sim F6X-C39 \\sim F5-C39 \\sim F4X-C39 \\sim F6-C39
 with sigma of 0.01
 C65A-C64 \\sim C65-C64
 with sigma of 0.02
 C66-C65 \\sim C66A-C65A
 with sigma of 0.02
 C67-C66 \\sim C67A-C66A
 with sigma of 0.02
 O5-C67 \\sim O5-C67A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F6X)
Uanis(C65A) = Uanis(C65)
Uanis(C66) = Uanis(C66A)
Uanis(C67) = Uanis(C67A)
4. Rigid body (RIGU) restrains
 C34, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F5, F6, F5X, F4X, F6X, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C64, C65, C66, C67, C67A, C66A, C65A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C68, C69, C70, C71
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F5X)=Sof(F4X)=Sof(F6X)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(H64C)=Sof(H64D)=Sof(C67A)=Sof(H67C)=Sof(H67D)=Sof(C66A)=Sof(H66C)=
 Sof(H66D)=Sof(C65A)=Sof(H65C)=Sof(H65D)=1-FVAR(2)
 Sof(H64A)=Sof(H64B)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=
 Sof(C67)=Sof(H67A)=Sof(H67B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 B1(H1A)
6.b Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C64(H64C,H64D), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,
 H67B), C67A(H67C,H67D), C66A(H66C,H66D), C65A(H65C,H65D), C69(H69A,H69B),
 C70(H70A,H70B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C8(H8), C9(H9), C15(H15), C16(H16), C24(H24), C25(H25),
 C26(H26), C27(H27), C33(H33), C35(H35), C37(H37), C41(H41), C43(H43), C45(H45),
  C49(H49), C51(H51), C53(H53), C57(H57), C59(H59), C61(H61)
6.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C68(H68A,H68B,H68C), C71(H71A,H71B,H71C)
;
_shelx_res_checksum              22941
_shelx_hkl_checksum              8220
_shelx_fab_checksum              49992
_olex2_submission_special_instructions 'No special instructions were received'