NMR-based investigations of acyl-functionalized piperazines concerning their conformational behavior in solution
Wodtke, Robert; Steinberg, Janine; Köckerling, Martin; Löser, Reik; Mamat, Constantin; RSC Advances 8 (2018) 40921–; doi:10.1039/C8RA09152H

data_7231958
_publ_section_title
;
 NMR-based investigations of acyl-functionalized piperazines concerning
 their conformational behavior in solution
;
_journal_issue                   71
_journal_name_full               'RSC Advances'
_journal_page_first              40921
_journal_paper_doi               10.1039/C8RA09152H
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C17 H16 Br N3 O3'
_chemical_formula_sum            'C17 H16 Br N3 O3'
_chemical_formula_weight         390.24
_chemical_melting_point_gt       405
_chemical_melting_point_lt       407
_chemical_name_systematic
;
1-(3-Bromobenzoyl)-4-(4-nitrophenyl)piperazine
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             april-19-2018
_audit_creation_method           'ciftab-2016(M. K\"ockerling, 2016)'
_audit_update_record
;
2018-04-19 deposited with the CCDC.
2018-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.67(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.842(3)
_cell_length_b                   25.300(9)
_cell_length_c                   8.024(3)
_cell_measurement_reflns_used    8859
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.606
_cell_volume                     1586.7(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            35509
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.375
_diffrn_reflns_theta_min         2.606
_exptl_absorpt_coefficient_mu    2.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker-Nonius SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.095
_exptl_transmission_factor_max   0.74570
_exptl_transmission_factor_min   0.62880
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0030P)^2^+4.4635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2674
_reflns_number_total             3910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra09152h2.cif
_cod_data_source_block           CM589C
_cod_original_cell_volume        1586.7(9)
_cod_database_code               7231958
_shelx_estimated_absorpt_t_min   0.744
_shelx_estimated_absorpt_t_max   0.789
_shelxl_version_number           2014-1
_shelx_res_checksum              58624
_shelx_hkl_checksum              6693