Unravelling conformational and crystal packing preferences of cyclohexane-5-spirohydantoin derivatives incorporating a halogenated benzoyl group
Lazić, Anita; Radovanović, Lidija; Gak Simić, Kristina; Rogan, Jelena; Janjić, Goran; Trišović, Nemanja; Đorđević, Ivana; CrystEngComm  (2022) –; doi:10.1039/D2CE00376G

data_7244961
_publ_section_title
;
 Unravelling conformational and crystal packing preferences of
 cyclohexane-5-spirohydantoin derivatives incorporating a halogenated
 benzoyl group
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00376G
_journal_year                    2022
_chemical_formula_moiety         'C15 H15 Br N2 O3'
_chemical_formula_sum            'C15 H15 Br N2 O3'
_chemical_formula_weight         351.2
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2022-03-04 deposited with the CCDC.	2022-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                106.54(3)
_cell_angle_beta                 100.99(3)
_cell_angle_gamma                91.53(3)
_cell_formula_units_Z            2
_cell_length_a                   6.6479(13)
_cell_length_b                   10.089(2)
_cell_length_c                   12.122(2)
_cell_measurement_reflns_used    2735
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1040
_cell_measurement_theta_min      3.1400
_cell_volume                     762.3(3)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-2014 (Burla et al., 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3280
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11556
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         3.133
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.53
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.9158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                2112
_reflns_number_total             2789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00376g2.cif
_cod_data_source_block           2
_cod_original_cell_volume        762.2(3)
_cod_database_code               7244961