Syntheses and crystal structures of benzyl <i>N</i>'-[(<i>E</i>)-2-hydroxybenzylidene]hydrazinecarboxylate and benzyl <i>N</i>'-[(<i>E</i>)-5-bromo-2-hydroxybenzylidene]hydrazinecarboxylate
Vinaya; Basavaraju, Yeriyur B.; Lakshmana, Beliyaiah; Yathirajan, Hemmige S.; Parkin, Sean; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022009100

data_2244177
_publ_section_title
;
 Syntheses and crystal structures of benzyl
 <i>N</i>'-[(<i>E</i>)-2-hydroxybenzylidene]hydrazinecarboxylate and
 benzyl
 <i>N</i>'-[(<i>E</i>)-5-bromo-2-hydroxybenzylidene]hydrazinecarboxylate
;
_journal_coeditor_code           YK2176
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022009100
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C15 H13 Br N2 O3'
_chemical_formula_moiety         'C15 H13 Br N2 O3'
_chemical_formula_sum            'C15 H13 Br N2 O3'
_chemical_formula_weight         349.18
_chemical_name_systematic
;
Benzyl <i>N</i>'-[(<i>E</i>)-5-bromo-2-hydroxybenzylidene]hydrazinecarboxylate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                90
_cell_angle_beta                 94.485(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.904(2)
_cell_length_b                   11.1207(6)
_cell_length_c                   9.0648(7)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.34
_cell_volume                     2804.3(3)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_publication_material
;
<i>CIFFIX</i> (Parkin, 2013) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            36145
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_min         1.972
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.943
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al</i>., 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0240P)^2^+0.4336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                5004
_reflns_number_total             6401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2176sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2244177
_shelx_estimated_absorpt_t_min   0.539
_shelx_estimated_absorpt_t_max   0.867
_shelx_hkl_checksum              55303
_shelx_res_checksum              8367
_cod_database_fobs_code 2244177