Multielectron C-H photoactivation with an Sb(v) oxo corrole.
Lemon, Christopher M.; Maher, Andrew G.; Mazzotti, Anthony R.; Powers, David C.; Gonzalez, Miguel I.; Nocera, Daniel G.; Chemical communications (Cambridge, England) 56 (2020) 5247–5250; doi:10.1039/c9cc09892e

data_7126283
_publ_section_title
;
 Multielectron C-H photoactivation with an Sb(v) oxo corrole.
;
_journal_issue                   39
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5247
_journal_page_last               5250
_journal_paper_doi               10.1039/c9cc09892e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C78 H30 F20 N8 O6 Sb2, 4(C7 H8)'
_chemical_formula_sum            'C106 H62 F20 N8 O6 Sb2'
_chemical_formula_weight         2167.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-02-13
_audit_creation_method
;
Olex2 1.3
(compiled 2019.11.21 svn.r41b79517 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-09 deposited with the CCDC.	2020-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.277(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7806(17)
_cell_length_b                   19.611(2)
_cell_length_c                   32.180(4)
_cell_measurement_reflns_used    3107
_cell_measurement_temperature    99.98
_cell_measurement_theta_max      18.414
_cell_measurement_theta_min      2.443
_cell_volume                     9178.1(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1222
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38130
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        18.507
_diffrn_reflns_theta_max         18.507
_diffrn_reflns_theta_min         1.221
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0807 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.8407.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4336
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.066
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.148
_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     1247
_refine_ls_number_reflns         6846
_refine_ls_number_restraints     1931
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0818
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1409P)^2^+116.7862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4599
_reflns_number_total             6846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09892e2.cif
_cod_data_source_block           dcp1428_sq
_cod_depositor_comments          'Adding full bibliography for 7126283.cif.'
_cod_original_cell_volume        9177.8(19)
_cod_database_code               7126283
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.934
_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. Restrained distances
 C106-C100
 1.51 with sigma of 0.02
 C1B-C107
 1.51 with sigma of 0.02
 C99-C93
 1.51 with sigma of 0.02
 C105-C106 \\sim C101-C106
 with sigma of 0.02
3. Restrained planarity
 C103, C102, C101, C100, C105, C104, C106
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N8 \\sim N5 \\sim N6 \\sim N1 \\sim N2 \\sim N7 \\sim N4 \\sim N3 \\sim C43
\\sim C19 \\sim C58 \\sim C47 \\sim C4 \\sim C48 \\sim C54 \\sim C18 \\sim C57
\\sim C41 \\sim C55 \\sim C2 \\sim C40 \\sim C13 \\sim C7 \\sim C5 \\sim C15
\\sim C53 \\sim C44 \\sim C52 \\sim C10 \\sim C1 \\sim C49 \\sim C46 \\sim C14
\\sim C16 \\sim C50 \\sim C8 \\sim C45 \\sim C11 \\sim C51 \\sim C9 \\sim C12
\\sim C56 \\sim C42 \\sim C3 \\sim C6 \\sim C17: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C82 \\sim C83 \\sim C79 \\sim C81 \\sim C85 \\sim C84 \\sim C80: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C72 \\sim O5 \\sim C71 \\sim O6 \\sim C69 \\sim C68 \\sim C67 \\sim C66 \\sim
C65 \\sim C70: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O3 \\sim O4 \\sim C32 \\sim C29 \\sim C27 \\sim C28 \\sim C26 \\sim C30 \\sim
C31 \\sim C33: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F5 \\sim F1 \\sim F4 \\sim F3 \\sim F2 \\sim C23 \\sim C24 \\sim C25 \\sim C21
\\sim C20 \\sim C22: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C96 \\sim C97 \\sim C98 \\sim C93 \\sim C94 \\sim C95 \\sim C99: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C91 \\sim C86 \\sim C87 \\sim C90 \\sim C92 \\sim C88 \\sim C89: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C106 \\sim C100 \\sim C105 \\sim C104 \\sim C103 \\sim C102 \\sim C101 \\sim
C107 \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C44) = Uanis(C43)
Uanis(N6) = Uanis(N5) = Uanis(N8) = Uanis(N7)
Uanis(N3) = Uanis(N4) = Uanis(N1) = Uanis(N2)
5. Rigid body (RIGU) restrains
 N8, N5, N6, N1, N2, N7, N4, N3, C43, C19, C58, C47, C4, C48, C54, C18, C57,
 C41, C55, C2, C40, C13, C7, C5, C15, C53, C44, C52, C10, C1, C49, C46, C14,
 C16, C50, C8, C45, C11, C51, C9, C12, C56, C42, C3, C6, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C82, C83, C79, C81, C85, C84, C80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C72, O5, C71, O6, C69, C68, C67, C66, C65, C70
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O4, C32, C29, C27, C28, C26, C30, C31, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F5, F1, F4, F3, F2, C23, C24, C25, C21, C20, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F20, F16, F17, F19, F18, C74, C73, C75, C78, C76, C77
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F6, F10, F9, F7, F8, C35, C37, C34, C39, C36, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F15, F11, F12, F14, F13, C59, C64, C63, C60, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C96, C97, C98, C93, C94, C95, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C91, C86, C87, C90, C92, C88, C89
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C102, C106, C100, C105, C101, C104, C103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1F, C107, C1B, C1A, C1C, C1D, C1E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C106(0.47) H10A(0.47) H10B(0.47) H10C(0.47) C100(0.47) C105(0.47)
 H105(0.47) C104(0.47) H104(0.47) C103(0.47) H103(0.47) C102(0.47) H102(0.47)
 C101(0.47) H101(0.47) C107(0.53) H10D(0.53) H10E(0.53) H10F(0.53) C1A(0.53)
 H1A(0.53) C1B(0.53) C1C(0.53) H1C(0.53) C1D(0.53) H1D(0.53) C1E(0.53)
 H1E(0.53) C1F(0.53) H1F(0.53)
7.a Aromatic/amide H refined with riding coordinates:
 C41(H41), C69(H69), C67(H67), C66(H66), C70(H70), C55(H55), C2(H2), C56(H56),
 C7(H7), C42(H42), C46(H46), C16(H16), C50(H50), C45(H45), C3(H3), C11(H11),
 C51(H51), C6(H6), C17(H17), C27(H27), C28(H28), C12(H12), C30(H30), C31(H31),
 C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C91(H91), C87(H87), C90(H90),
  C88(H88), C96(H96), C97(H97), C98(H98), C94(H94), C95(H95), C89(H89),
 C105(H105), C104(H104), C103(H103), C102(H102), C101(H101), C1A(H1A), C1C(H1C),
  C1D(H1D), C1E(H1E), C1F(H1F)
7.b Fitted hexagon refined as free rotating group:
 C69(C68,C67,C66,C65,C70), C79(C80,C81,C82,C83,C84), C96(C97,C98,C93,C94,C95),
 C100(C105,C104,C103,C102,C101), C1A(C1B,C1C,C1D,C1E,C1F)
7.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C72(H72A,H72B,H72C), C85(H85A,H85B,H85C), C92(H92A,H92B,
 H92C), C99(H99A,H99B,H99C), C106(H10A,H10B,H10C), C107(H10D,H10E,H10F)
;
_shelx_res_checksum              67489
_shelx_fab_checksum              8151
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'