Six 1-halobenzoyl-4-(2-methoxyphenyl)piperazines having <i>Z</i>' values of one, two or four; disorder, pseudosymmetry, twinning and supramolecular assembly in one, two or three dimensions
Harish Chinthal, Chayanna; Kavitha, Channappa N.; Yathirajan, Hemmige S.; Foro, Sabine; Glidewell, Christopher; Acta Crystallographica Section E 77 (2021) 5–13; doi:10.1107/S2056989020015649

data_2243696
_publ_section_title
;
 Six 1-halobenzoyl-4-(2-methoxyphenyl)piperazines having <i>Z</i>' values
 of one, two or four; disorder, pseudosymmetry, twinning and
 supramolecular assembly in one, two or three dimensions
;
_journal_coeditor_code           HB7954
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              5
_journal_page_last               13
_journal_paper_doi               10.1107/S2056989020015649
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C18 H19 I N2 O2'
_chemical_formula_moiety         'C18 H19 I N2 O2'
_chemical_formula_sum            'C18 H19 I N2 O2'
_chemical_formula_weight         422.25
_chemical_name_systematic
;
1-(3-Iodobenzoyl)-4-(2-methoxyphenyl)piperazine
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.4528(4)
_cell_length_b                   17.1306(9)
_cell_length_c                   27.9030(10)
_cell_measurement_reflns_used    7668
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.886
_cell_measurement_theta_min      2.790
_cell_volume                     3562.4(3)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13774
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysalisRed; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.689
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1728 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.456(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0552P)^2^+0.7763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                5048
_reflns_number_total             7653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7954sup1.cif
_cod_data_source_block           V
_cod_database_code               2243696
_cod_database_fobs_code          2243696
_shelx_estimated_absorpt_t_min   0.562
_shelx_estimated_absorpt_t_max   0.737
_shelx_hkl_checksum              7092
_shelx_res_checksum              67045
_shelxl_version_number           2.014