Hypervalent iodine promoted the synthesis of cycloheptatrienes and cyclopropanes
Yuan, Da-Fu; Wang, Zi-Chen; Geng, Rui-Sen; Ren, Guang-Yi; Wright, James S.; Ni, Shao-Fei; Li, Ming; Wen, Li-Rong; Zhang, Lin-Bao; Chemical Science 13 (2022) 478–485; doi:10.1039/D1SC05429E

data_1565604
_publ_section_title
;
 Hypervalent iodine promoted the synthesis of cycloheptatrienes and
 cyclopropanes
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              478
_journal_page_last               485
_journal_paper_doi               10.1039/D1SC05429E
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C18 H14 Br N O2'
_chemical_formula_sum            'C18 H14 Br N O2'
_chemical_formula_weight         356.21
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2018-10-19 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13497
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         75.388
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_diffrn_source                   'Rotating-anode X-ray tube'
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             720
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_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.189
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_refine_ls_extinction_method     none
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.7326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2707
_reflns_number_total             2934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05429e2.cif
_cod_data_source_block           tx32
_cod_depositor_comments
'Adding full bibliography for 1565604--1565606.cif.'
_cod_database_code               1565604
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.528
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18)
;
_shelx_res_checksum              61341
_shelx_hkl_checksum              45857
_olex2_submission_special_instructions 'No special instructions were received'