The unusual (syn-/anti-)2 conformation of a dimethoxypyrimidyl-based tennimide
Mocilac, Pavle; Pohl, Fabian; Gallagher, John F.; Acta Crystallographica Section E Crystallographic Communications 79 (2023) –; doi:10.1107/S2056989023006837

data_2022845
_publ_section_title
;
 The unusual (syn-/anti-)2 conformation of a dimethoxypyrimidyl-based
 tennimide
;
_journal_coeditor_code           EX2073
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989023006837
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C52 H40 N16 O16, 0.167H2 O'
_chemical_formula_moiety         'C52 H40 N16 O16, 0.167(H2 O)'
_chemical_formula_sum            'C52 H40.33 N16 O16.17'
_chemical_formula_weight         1148.02
_chemical_name_common            Dimethoxypyrimidyltennimide
_chemical_name_systematic
;
3,11,19,27-Tetrakis(4,6-dimethoxypyrimidin-2-yl)-3,11,19,27,33,34,35,36-\
octaazapentacyclo[27.3.1.1^5,9^.1^13,17^.1^21,25^]hexatriaconta-\
1(33),5,7,9(36),13(35),14,16,21(34),22,24,29,31-dodecaen-\
2,4,10,12,18,20,26,28-octone 0.167-hydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
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_atom_sites_solution_secondary   geom
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_a                   18.8065(10)
_cell_length_b                   10.0745(6)
_cell_length_c                   28.847(3)
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_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      63.57
_cell_measurement_theta_min      2.80
_cell_volume                     5465.5(7)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
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CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020) and Mercury (Macrae <i>et al.</i>,  2020)
;
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;
<i>SHELXL14/6</i> (Sheldrick, 2015b)
;
_computing_structure_refinement
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<i>SHELXL14/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT14/6</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14675
_diffrn_reflns_theta_full        61.080
_diffrn_reflns_theta_max         63.639
_diffrn_reflns_theta_min         3.064
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
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_exptl_absorpt_process_details
;
(<i>ABSFAC</i>; Clark & Reid, 1998)
;
_exptl_crystal_colour            colourless
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_exptl_crystal_F_000             2374.7
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.178
_refine_ls_extinction_coef       0.00055(7)
_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   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0686P)^2^+1.3472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                3036
_reflns_number_total             4439
_reflns_threshold_expression     I>2\s(I)
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_cod_data_source_block           I
_cod_original_cell_volume        5465.6(7)
_cod_database_code               2022845
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.969
_shelx_hkl_checksum              11692
_shelx_res_checksum              48758
_shelxl_version_number           2014/6
_cod_database_fobs_code 2022845