Crystal structures of 2-[3,5-bis(bromomethyl)-2,4,6-triethylbenzyl]isoindoline-1,3-dione and 2-{5-(bromomethyl)-3-[(1,3-dioxoisoindolin-2-yl)methyl]-2,4,6-triethylbenzyl}isoindoline-1,3-dione
Stapf, Manuel; Leibiger, Betty; Schwarzer, Anke; Mazik, Monika; Acta Crystallographica Section E 77 (2021) 919–923; doi:10.1107/S205698902100788X

data_2244191
_publ_section_title
;
 Crystal structures of
 2-[3,5-bis(bromomethyl)-2,4,6-triethylbenzyl]isoindoline-1,3-dione and
 2-{5-(bromomethyl)-3-[(1,3-dioxoisoindolin-2-yl)methyl]-2,4,6-triethylbenzyl}isoindoline-1,3-dione
;
_journal_coeditor_code           ZQ2264
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              919
_journal_page_last               923
_journal_paper_doi               10.1107/S205698902100788X
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C31 H29 Br N2 O4'
_chemical_formula_moiety         'C31 H29 Br N2 O4'
_chemical_formula_sum            'C31 H29 Br N2 O4'
_chemical_formula_weight         573.47
_chemical_name_systematic
2-{5-(Bromomethyl)-3-[(1,3-dioxoisoindolin-2-yl)methyl]-2,4,6-triethylbenzyl}isoindoline-1,3-dione
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 109.168(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.899(2)
_cell_length_b                   12.9748(15)
_cell_length_c                   16.763(3)
_cell_measurement_reflns_used    3744
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.02
_cell_volume                     2650.0(7)
_computing_cell_refinement
;
X-AREA (Stoe, 2009)
;
_computing_data_collection
;
X-AREA (Stoe, 2009)
;
_computing_data_reduction
;
X-RED (Stoe, 2009)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008)
;
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 2012), <i>publCIF</i> (Westrip, 2010)
and <i>shelXle</i>
(H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      153
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1151
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26391
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.742
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  0.8444
_exptl_absorpt_correction_T_min  0.6952
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       piece
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.669
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0406P)^2^+4.7828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                3442
_reflns_number_total             4941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq2264sup1.cif
_cod_data_source_block           2
_cod_original_cell_volume        2649.9(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2244191
_shelx_estimated_absorpt_t_min   0.763
_shelx_estimated_absorpt_t_max   0.796
_shelx_hkl_checksum              48843
_shelx_res_checksum              25704
_cod_database_fobs_code 2244191