Crystal structure of (E)-N-(2-(benzylamino)-2-oxo-1-(4-oxo-4H-chromen-3-yl)ethyl)-N-(4-bromophenyl)-3-chloroacrylamide hydrate, C27H22BrClN2O5
Meng, Jiang Ping; Lei, Jie; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 589–590; doi:10.1515/ncrs-2017-0346

data_8106224
_publ_section_title
;
 Crystal structure of
 (E)-N-(2-(benzylamino)-2-oxo-1-(4-oxo-4H-chromen-3-yl)ethyl)-N-(4-bromophenyl)-3-chloroacrylamide
 hydrate, C27H22BrClN2O5
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              589
_journal_page_last               590
_journal_paper_doi               10.1515/ncrs-2017-0346
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C27 H20 Br Cl N2 O4, H2 O'
_chemical_formula_sum            'C27 H22 Br Cl N2 O5'
_chemical_formula_weight         569.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                85.944(7)
_cell_angle_beta                 84.882(6)
_cell_angle_gamma                89.932(6)
_cell_formula_units_Z            2
_cell_length_a                   6.8549(4)
_cell_length_b                   13.2863(12)
_cell_length_c                   14.3690(13)
_cell_measurement_reflns_used    2359
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.8340
_cell_measurement_theta_min      3.3360
_cell_volume                     1300.18(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -32.00   52.00   1.0000    3.7500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669   57.0000  120.0000 84

  2 omega  -26.00    4.00   1.0000    3.7500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -19.0000  -60.0000 30

  3 omega  -22.00   24.00   1.0000    3.7500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -99.0000    0.0000 46

  4 omega  -24.00   17.00   1.0000    3.7500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -99.0000  150.0000 41

  5 omega  -32.00   -5.00   1.0000    3.7500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669   57.0000 -120.0000 27

  6 omega   13.00   52.00   1.0000    3.7500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669   57.0000 -120.0000 39

  7 omega  -28.00   54.00   1.0000    3.7500
omega____ theta____ kappa____ phi______ frames
    -      -14.9669   38.0000    0.0000 82

  8 omega   53.00   88.00   1.0000    3.7500
omega____ theta____ kappa____ phi______ frames
    -       16.8419 -178.0000    0.0000 35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0265553000
_diffrn_orient_matrix_UB_12      0.0324945000
_diffrn_orient_matrix_UB_13      0.0360908000
_diffrn_orient_matrix_UB_21      0.0168247000
_diffrn_orient_matrix_UB_22      -0.0395157000
_diffrn_orient_matrix_UB_23      0.0341400000
_diffrn_orient_matrix_UB_31      0.0990189000
_diffrn_orient_matrix_UB_32      0.0157183000
_diffrn_orient_matrix_UB_33      -0.0007799000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.984
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description
;
;
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0830P)^2^+0.5697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1841
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3325
_reflns_number_total             5316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0346_suppl.cif
_cod_data_source_block           s7_lj
_cod_database_code               8106224
_chemical_oxdiff_formula         c12h12n2o3
_shelx_estimated_absorpt_t_max   0.673
_shelx_estimated_absorpt_t_min   0.584
_exptl_absorpt_special_details   block
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C9(H9), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27)
;
_olex2_submission_special_instructions 'No special instructions were received'