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_1549287
_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
'C57 H78 B Co F3 N8 O3 S, C32 H12 B F24, C4 H10 O'
_chemical_formula_sum            'C93 H100 B2 Co F27 N8 O4 S'
_chemical_formula_weight         2019.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4930(17)
_cell_length_b                   22.3378(19)
_cell_length_c                   38.715(3)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.05
_cell_measurement_theta_min      2.31
_cell_volume                     18587(3)
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2018/1 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  D8Venture
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1273
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            251224
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.816
_diffrn_reflns_theta_max         24.816
_diffrn_reflns_theta_min         2.103
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0984 before and 0.0654 after correction. 
The Ratio of minimum to maximum transmission is 0.9055. 
;
_exptl_crystal_colour            'bluish violet'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             8336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.919
_refine_diff_density_min         -2.371
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1213
_refine_ls_number_reflns         16006
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.1073
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1262P)^2^+167.7536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2609
_refine_ls_wR_factor_ref         0.2964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10634
_reflns_number_total             16006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01167b2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1549282--1549287.cif.'
_cod_database_code               1549287
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.897
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F5-F4
 2.1 with sigma of 0.005
 F6-F5
 2.1 with sigma of 0.005
 F6-F4
 2.1 with sigma of 0.005
 F5-C64 = F4-C64 = F6-C64
 1.32 with sigma of 0.001
 F8-C65
 1.32 with sigma of 0.02
 F8-F7
 2.1 with sigma of 0.02
 F9-F7
 2.1 with sigma of 0.02
 F9-F8
 2.1 with sigma of 0.02
 F8A-F7A
 2.1 with sigma of 0.02
 F7A-F9A
 2.1 with sigma of 0.02
 F8A-F9A
 2.1 with sigma of 0.02
 C65-C62
 1.45 with sigma of 0.02
 C81-C76 \\sim C64-C60
 with sigma of 0.001
 F5-C64 \\sim F6-C64 \\sim F18-C81 \\sim F16-C81 \\sim F17-C81
 with sigma of 0.001
 C81-C76 \\sim C65-C62
 with sigma of 0.001
 C80-C78 \\sim C88-C84 \\sim C89-C86 \\sim C73-C70 \\sim C81-C76
 with sigma of 0.02
 F8A-C65 \\sim F8-C65 \\sim F7A-C65 \\sim F7-C65 \\sim F9A-C65 \\sim F9-C65
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C64) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 F7, F8, C65, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F8A)=Sof(F7A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Fixed Uiso: F4(0.1)
6.a Ternary CH refined with riding coordinates:
 C8(H8A), C10(H10), C12(H12), C22(H22), C24(H24), C26(H26), C35(H35), C37(H37),
  C39(H39), C50(H50), C52(H52), C54(H54), B1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C13(H13A,
 H13B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B),
 C25(H25A,H25B), C27(H27A,H27B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C36(H36A,H36B), C38(H38A,H38B), C40(H40A,H40B), C47(H47A,H47B), C48(H48A,
 H48B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,H53B), C55(H55A,H55B),
 C91(H91A,H91B), C92(H92A,H92B)
6.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N8(H8), C2(H2), C16(H16), C44(H44), C59(H59), C61(H61), C63(H63),
 C67(H67), C69(H69), C71(H71), C75(H75), C77(H77), C79(H79), C83(H83), C85(H85),
  C87(H87)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C56(H56A,H56B,
 H56C), C90(H90A,H90B,H90C), C93(H93A,H93B,H93C)
;
_shelx_res_checksum              42990
_shelx_hkl_checksum              59096
_olex2_submission_special_instructions 'No special instructions were received'