Pseudo three-component approach to coumarin-annulated azepines: synthesis of coumarin[3,4-b]azepines
Manjappa, Kiran B.; Peng, Yu-Ting; Liou, Teau-Jiuan; Yang, Ding-Yah; RSC Adv. 7 (2017) 45269–; doi:10.1039/C7RA09289J

data_7229228
_publ_section_title
;
 Pseudo three-component approach to coumarin-annulated azepines: synthesis
 of coumarin[3,4-b]azepines
;
_journal_issue                   72
_journal_name_full               'RSC Adv.'
_journal_page_first              45269
_journal_paper_doi               10.1039/C7RA09289J
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C25 H15 Br2 N O2'
_chemical_formula_sum            'C25 H15 Br2 N O2'
_chemical_formula_weight         521.20
_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_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-10 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                68.214(2)
_cell_angle_beta                 87.658(2)
_cell_angle_gamma                69.9597(19)
_cell_formula_units_Z            2
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_cell_length_b                   11.4244(6)
_cell_length_c                   11.4731(7)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.405
_cell_measurement_theta_min      3.192
_cell_volume                     1048.01(11)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19733
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.410
_diffrn_reflns_theta_min         3.192
_exptl_absorpt_coefficient_mu    3.890
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.4600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.590
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_refine_diff_density_max         1.872
_refine_diff_density_min         -0.802
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0838
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_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^)+(0.0708P)^2^+7.7818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3444
_reflns_number_total             4268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra09289j2.cif
_cod_data_source_block           bmk4553
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7229228
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.207
_shelx_estimated_absorpt_t_max   0.525
_shelx_res_checksum              72275