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_7231959
_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       460
_chemical_melting_point_lt       462
_chemical_name_systematic
;
1-(4-Bromobenzoyl)-4-(4-nitrophenyl)piperazine

;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             february-24-2018
_audit_creation_method           'ciftab-2016(M. K\"ockerling, 2016)'
_audit_update_record
;
2018-02-24 deposited with the CCDC.
2018-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.727(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.379(2)
_cell_length_b                   11.788(2)
_cell_length_c                   17.806(2)
_cell_measurement_reflns_used    7876
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.443
_cell_measurement_theta_min      2.1995
_cell_volume                     3258.1(8)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33067
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         33.778
_diffrn_reflns_theta_min         2.169
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker-Nonius SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    none
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.110
_exptl_transmission_factor_max   0.74670
_exptl_transmission_factor_min   0.57790
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         6516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.7557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3848
_reflns_number_total             6516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra09152h2.cif
_cod_data_source_block           PW108
_cod_original_cell_volume        3257.8(7)
_cod_database_code               7231959
_shelx_estimated_absorpt_t_min   0.592
_shelx_estimated_absorpt_t_max   0.767
_shelxl_version_number           2014-1
_shelx_res_checksum              29400
_shelx_hkl_checksum              25083