Crystal structure of 2-(2,2,6,6-tetramethylpiperidin-4-yl)-6-[(2,2,6,6-tetramethylpiperidin-4-yl)amino]-1<i>H</i>-benz[<i>de</i>]isoquinoline-1,3(2<i>H</i>)-dione
Pollock, Alicia A.; Huther, Holly A.; Birch, Cole M.; Reinheimer, Eric W.; Lewis, David E.; Gerlach, Deidra L.; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022010374

data_2244201
_publ_section_title
;
 Crystal structure of
 2-(2,2,6,6-tetramethylpiperidin-4-yl)-6-[(2,2,6,6-tetramethylpiperidin-4-yl)amino]-1<i>H</i>-benz[<i>de</i>]isoquinoline-1,3(2<i>H</i>)-dione
;
_journal_coeditor_code           MW2192
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022010374
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C30 H42 N4 O2'
_chemical_formula_moiety         'C30 H42 N4 O2'
_chemical_formula_sum            'C30 H42 N4 O2'
_chemical_formula_weight         490.67
_chemical_name_common            'bis-TMP naphthalimide'
_chemical_name_systematic
2-(2,2,6,6-Tetramethylpiperidin-4-yl)-6-[(2,2,6,6-tetramethylpiperidin-4-yl)amino]-1<i>H</i>-benz[<i>de</i>]isoquinoline-1,3(2<i>H</i>)-dione
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0297(7)
_cell_length_b                   14.6357(7)
_cell_length_c                   32.763(2)
_cell_measurement_reflns_used    6091
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5230
_cell_measurement_theta_min      2.1370
_cell_volume                     5768.4(6)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT  (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            80396
_diffrn_reflns_theta_full        25.162
_diffrn_reflns_theta_max         25.162
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlisPro; Rigaku OD, 2022;
analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.563
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.148
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2016/6 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5164
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0686P)^2^+1.5942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                3812
_reflns_number_total             5164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2192sup1.cif
_cod_data_source_block           I
_cod_database_code               2244201
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.987
_cod_database_fobs_code 2244201