BrØnsted Acid Mediated Intramolecular Cyclopropane Ring Expansion/[4+2]-Cycloaddition
Li, Jian; zhu, shang-rong; Xu, Qiuneng; Liu, Li; Yan, Shenghu; Organic & Biomolecular Chemistry  (2019) –; doi:10.1039/C9OB02379H

data_7157208
_publ_section_title
;
 Br\/Onsted Acid Mediated Intramolecular Cyclopropane Ring
 Expansion/[4+2]-Cycloaddition
;
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/C9OB02379H
_journal_year                    2019
_chemical_formula_sum            'C24 H17 Br I N O2'
_chemical_formula_weight         558.20
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-22 deposited with the CCDC.	2019-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.1680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4658(4)
_cell_length_b                   15.2404(4)
_cell_length_c                   10.0603(3)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      53.99
_cell_measurement_theta_min      2.96
_cell_volume                     1992.69(10)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17028
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.993
_diffrn_reflns_theta_min         2.958
_exptl_absorpt_coefficient_mu    10.332
_exptl_absorpt_correction_T_max  0.3012
_exptl_absorpt_correction_T_min  0.0787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.020
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0595P)^2^+5.0666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3223
_reflns_number_total             3655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob02379h2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7157208
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.370
_shelx_estimated_absorpt_t_max   0.492
_shelx_res_checksum              21793