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_7231957
_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         'C18 H16 F2 N2 O2'
_chemical_formula_sum            'C18 H16 F2 N2 O2'
_chemical_formula_weight         330.33
_chemical_name_systematic
;
N,N'-Bis-(4F-fluorobenzoyl)-piperazine
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             january-14-2018
_audit_creation_method           'ciftab-2016(M. K\"ockerling, 2016)'
_audit_update_record
;
2018-01-14 deposited with the CCDC.
2018-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.313(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.5750(4)
_cell_length_b                   10.4009(7)
_cell_length_c                   11.2622(7)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      46.729
_cell_measurement_theta_min      2.6895
_cell_volume                     755.21(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      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44151
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         46.731
_diffrn_reflns_theta_min         2.690
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker-Nonius SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    none
_exptl_crystal_description       cube
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.210
_exptl_transmission_factor_max   0.74920
_exptl_transmission_factor_min   0.66450
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         6803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0781P)^2^+0.1170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4519
_reflns_number_total             6803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra09152h2.cif
_cod_data_source_block           CM611
_cod_database_code               7231957
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2014-1
_shelx_res_checksum              34430
_shelx_hkl_checksum              70659