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_1549282
_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         'C43 H58 B Co F3 N6 O3 S'
_chemical_formula_sum            'C43 H58 B Co F3 N6 O3 S'
_chemical_formula_weight         865.75
_chemical_name_systematic        CoTpAd,MeOTf
_chemical_properties_physical    Air-sensitive
_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   mixed
_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                94.871(2)
_cell_angle_beta                 98.674(2)
_cell_angle_gamma                92.305(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3925(6)
_cell_length_b                   16.9868(8)
_cell_length_c                   21.7195(11)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.35
_cell_volume                     4134.1(4)
_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_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  D8Venture
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            183013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.399
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.0921 before and 0.0553 after correction. 
The Ratio of minimum to maximum transmission is 0.9438. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       block
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         20681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0508P)^2^+2.8636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15143
_reflns_number_total             20681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01167b2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1549282--1549287.cif.'
_cod_database_code               1549282
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.833
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C9(H9), C12(H12), C21(H21), C23(H23), C26(H26), C35(H35), C37(H37),
 C41(H41), C49(H49), C51(H51), C54(H54), C63(H63), C66(H66), C69(H69), C77(H77),
  C79(H79), C83(H83)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B),
 C14(H14A,H14B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B),
  C27(H27A,H27B), C28(H28A,H28B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B), C42(H42A,H42B), C48(H48A,H48B),
 C50(H50A,H50B), C52(H52A,H52B), C53(H53A,H53B), C55(H55A,H55B), C56(H56A,H56B),
  C62(H62A,H62B), C64(H64A,H64B), C65(H65A,H65B), C67(H67A,H67B), C68(H68A,
 H68B), C70(H70A,H70B), C76(H76A,H76B), C78(H78A,H78B), C80(H80A,H80B),
 C81(H81A,H81B), C82(H82A,H82B), C84(H84A,H84B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C31(H31), C45(H45), C59(H59), C73(H73)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C43(H43A,H43B,
 H43C), C57(H57A,H57B,H57C), C71(H71A,H71B,H71C)
;
_shelx_res_checksum              16317
_shelx_hkl_checksum              47496
_olex2_submission_special_instructions 'No special instructions were received'