Crystal structure and Hirshfeld analysis of di-<i>tert</i>-butyl 2,2'-[(ethylazanediyl)bis(methylene)]bis(1<i>H</i>-pyrrole-1-carboxylate)
Kvyatkovskaya, Elizaveta A.; Atioğlu, Zeliha; Akkurt, Mehmet; Epifanova, Polina P.; Valchuk, Karina S.; Khrustalev, Victor N.; Bhattarai, Ajaya; Acta Crystallographica Section E 76 (2020) 1827–1831; doi:10.1107/S2056989020014966

data_2243675
_publ_section_title
;
 Crystal structure and Hirshfeld analysis of di-<i>tert</i>-butyl
 2,2'-[(ethylazanediyl)bis(methylene)]bis(1<i>H</i>-pyrrole-1-carboxylate)
;
_journal_coeditor_code           YZ2002
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1827
_journal_page_last               1831
_journal_paper_doi               10.1107/S2056989020014966
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C22 H33 N3 O4'
_chemical_formula_moiety         'C22 H33 N3 O4'
_chemical_formula_sum            'C22 H33 N3 O4'
_chemical_formula_weight         403.51
_chemical_name_systematic
;
Di-<i>tert</i>-butyl
2,2'-[(ethylazanediyl)bis(methylene)]bis(1<i>H</i>-pyrrole-1-carboxylate)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                100.95(3)
_cell_angle_beta                 109.41(3)
_cell_angle_gamma                111.12(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6579(19)
_cell_length_b                   11.798(2)
_cell_length_c                   12.216(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.0
_cell_measurement_theta_min      3.4
_cell_volume                     1146.3(7)
_computing_cell_refinement
;
<i>iMosflm</i> (Battye <i>et al.</i>,  2011)
;
_computing_data_collection
;
<i>Marccd</i> (Doyle, 2011)
;
_computing_data_reduction
;
<i>iMosflm</i> (Battye <i>et al.</i>,  2011)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.1543
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14236
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.479
_diffrn_reflns_theta_min         3.432
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Scala; Evans, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.319
_refine_ls_extinction_coef       0.039(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1797
_reflns_number_gt                3323
_reflns_number_total             4609
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           I
_cod_database_code               2243675
_cod_database_fobs_code          2243675
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              11965
_shelxl_version_number           2014/6