Synthesis and crystal structures of 1-benzoyl-4-(4-nitrophenyl)piperazine and 1-(4-bromobenzoyl)-4-phenylpiperazine at 90K
Archana, Sreeramapura D.; Kiran Kumar, Haruvegowda; Shankara Prasad, Holehundi J.; Yathirajan, Hemmige S.; Parkin, Sean; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022009008

data_2244179
_publ_section_title
;
 Synthesis and crystal structures of 1-benzoyl-4-(4-nitrophenyl)piperazine
 and 1-(4-bromobenzoyl)-4-phenylpiperazine at 90K
;
_journal_coeditor_code           TX2058
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022009008
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C17 H17 Br N2 O'
_chemical_formula_moiety         'C17 H17 Br N2 O'
_chemical_formula_sum            'C17 H17 Br N2 O'
_chemical_formula_weight         345.23
_chemical_name_systematic
;
1-(4-Bromobenzoyl)-4-phenylpiperazine
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_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                 98.6250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5162(3)
_cell_length_b                   6.1125(2)
_cell_length_c                   15.7249(5)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.62
_cell_volume                     714.28(4)
_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>SHELXTL</i> (Sheldrick, 2008) 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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         2.620
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.878
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       'slab cut from lath'
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.222
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1306 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.012(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         6918
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0158P)^2^+0.0999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                6410
_reflns_number_total             6918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2058sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2244179
_shelx_estimated_absorpt_t_min   0.432
_shelx_estimated_absorpt_t_max   0.846
_shelx_hkl_checksum              76395
_shelx_res_checksum              39843
_cod_database_fobs_code 2244179