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_1549285
_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
'C52 H71 B Co I N6 O3 S, C32 H12 B F24, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C84.5 H84 B2 Cl Co F24 I N6 O3 S'
_chemical_formula_weight         1962.53
_chemical_name_systematic        '[CoTpAd,MePhIO][BArF4]'
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2018-01-23 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                95.079(2)
_cell_angle_beta                 97.357(2)
_cell_angle_gamma                97.863(2)
_cell_formula_units_Z            4
_cell_length_a                   14.2995(9)
_cell_length_b                   16.0821(11)
_cell_length_c                   38.551(3)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.04
_cell_measurement_theta_min      2.32
_cell_volume                     8658.9(11)
_computing_cell_refinement       'SAINT V.8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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-2014/7 (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 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.1033
_diffrn_reflns_av_unetI/netI     0.1379
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            86794
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.070
_diffrn_reflns_theta_max         25.070
_diffrn_reflns_theta_min         2.164
_diffrn_source                   'micro-focus X-ray tube'
_diffrn_source_type              'INCOATEC ImuS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.5618
_exptl_absorpt_correction_T_min  0.4484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1158 before and 0.0586 after correction. 
The Ratio of minimum to maximum transmission is 0.7989. 
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       plate
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2310
_refine_ls_number_reflns         29336
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.0887
_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^)+(0.0377P)^2^+69.0859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17951
_reflns_number_total             29336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01167b2.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2019-07-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1549282--1549287.cif.
;
_cod_original_cell_volume        8658.9(10)
_cod_original_formula_moiety
'2(C52 H71 B Co I N6 O3 S), 2(C32 H12 B F24), C H2 Cl2'
_cod_original_formula_sum        'C169 H168 B4 Cl2 Co2 F48 I2 N12 O6 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     3925.06
_cod_database_code               1549285
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.799
_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. Uiso/Uaniso restraints and constraints
Uanis(C83) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C54) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uiso(C168) = Uiso(C1A)
3. Rigid body (RIGU) restrains
 C85, C86A, C87A, C88A, C89A, C90A, C91A, C92A, C93A, C94A, C86, C91, C93, C87,
  C92, C88, C94, C89, C90
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7, N8, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64, C65, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C85, C94A, C86A, C87A, C88A, C93A, C91A, C90A, C89A, C92A, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C90, C92, C87, C88, C89, C86, C85, C94, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C168, F46, F47, F48} sigma for 1-2: 0.01, 1-3: 0.02
as
{C1A, F46A, F47A, F48A}
5. Others
 Sof(F43A)=Sof(F44A)=Sof(F45A)=1-FVAR(1)
 Sof(F43)=Sof(F44)=Sof(F45)=FVAR(1)
 Sof(C1A)=Sof(F46A)=Sof(F47A)=Sof(F48A)=1-FVAR(2)
 Sof(C168)=Sof(F46)=Sof(F47)=Sof(F48)=FVAR(2)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
 Sof(C86A)=Sof(H86C)=Sof(H86D)=Sof(C87A)=Sof(H87A)=Sof(C88A)=Sof(H88C)=
 Sof(H88D)=Sof(C89A)=Sof(H89A)=Sof(C90A)=Sof(H90C)=Sof(H90D)=Sof(C91A)=
 Sof(H91A)=Sof(C92A)=Sof(H92C)=Sof(H92D)=Sof(C93A)=Sof(H93C)=Sof(H93D)=
 Sof(C94A)=Sof(H94C)=Sof(H94D)=1-FVAR(4)
 Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C91)=Sof(H91)=Sof(C93)=Sof(H93A)=Sof(H93B)=
 Sof(C87)=Sof(H87)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C88)=Sof(H88A)=Sof(H88B)=
 Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(C89)=Sof(H89)=Sof(C90)=Sof(H90A)=Sof(H90B)=
 FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C14(H14), C21(H21), C23(H23), C27(H27), C35(H35), C37(H37),
 C40(H40), B1(H1), C59(H59), C61(H61), C64(H64), C73(H73), C75(H75), C78(H78),
 B2(H2), C91(H91), C87(H87), C89(H89), C87A(H87A), C89A(H89A), C91A(H91A)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B),
 C13(H13A,H13B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B),
  C26(H26A,H26B), C28(H28A,H28B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,
 H38B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B), C58(H58A,H58B),
 C60(H60A,H60B), C62(H62A,H62B), C63(H63A,H63B), C65(H65A,H65B), C66(H66A,H66B),
  C72(H72A,H72B), C74(H74A,H74B), C76(H76A,H76B), C77(H77A,H77B), C79(H79A,
 H79B), C80(H80A,H80B), C169(H16A,H16B), C86(H86A,H86B), C93(H93A,H93B),
 C92(H92A,H92B), C88(H88A,H88B), C94(H94A,H94B), C90(H90A,H90B), C86A(H86C,
 H86D), C88A(H88C,H88D), C90A(H90C,H90D), C92A(H92C,H92D), C93A(H93C,H93D),
 C94A(H94C,H94D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C31(H31), C43(H43), C46(H46), C47(H47), C48(H48), C55(H55),
 C69(H69), C83(H83), C96(H96), C97(H97), C98(H98), C99(H99), C138(H138),
 C140(H140), C142(H142), C146(H146), C148(H148), C150(H150), C154(H154),
 C156(H156), C158(H158), C162(H162), C164(H164), C166(H166), C106(H106),
 C108(H108), C110(H110), C114(H114), C116(H116), C118(H118), C122(H122),
 C124(H124), C126(H126), C130(H130), C132(H132), C134(H134)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C67(H67A,
 H67B,H67C), C81(H81A,H81B,H81C), C102(H10C,H10D,H10E), C103(H10F,H10G,H10H),
 C104(H10I,H10J,H10K)
;
_shelx_res_checksum              86011
_shelx_hkl_checksum              70773
_shelx_fab_checksum              69156
_olex2_submission_special_instructions 'No special instructions were received'