Synthesis and crystal structure of 2,4,6,8-tetrakis(3,5-di-<i>tert</i>-butylphenoxy)pyrimido[5,4-<i>d</i>]pyrimidine: expansion of the Piedfort concept
Gall, James H.; MacNicol, David D.; MacSween, Ross; Frampton, Christopher S.; Acta Crystallographica Section E 75 (2019) 383–387; doi:10.1107/S2056989019002470

data_2242855
_publ_section_title
;
 Synthesis and crystal structure of
 2,4,6,8-tetrakis(3,5-di-<i>tert</i>-butylphenoxy)pyrimido[5,4-<i>d</i>]pyrimidine:
 expansion of the Piedfort concept
;
_journal_coeditor_code           HB7803
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              383
_journal_page_last               387
_journal_paper_doi               10.1107/S2056989019002470
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C62 H84 N4 O4'
_chemical_formula_moiety         'C62 H84 N4 O4'
_chemical_formula_sum            'C62 H84 N4 O4'
_chemical_formula_weight         949.33
_chemical_name_common
;
;
_chemical_name_systematic
2,4,6,8-Tetrakis(3,5-di-<i>tert</i>-butylphenoxy)pyrimido[5,4-<i>d</i>]pyrimidine
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 93.0666(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.48641(17)
_cell_length_b                   15.84310(14)
_cell_length_c                   39.4611(4)
_cell_measurement_reflns_used    22911
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      76.3170
_cell_measurement_theta_min      2.2310
_cell_volume                     11540.90(19)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2015) and <i>Mercury</i> (Macrae <i>et al</i>.,
2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), <i>Mercury</i> (Macrae <i>et al</i>.,
2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXD2014 (Schneider & Sheldrick, 2002)
;
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 5.2921
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            55767
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.494
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       Block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1461
_refine_ls_number_reflns         23570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0575P)^2^+4.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                19544
_reflns_number_total             23570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7803sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        11540.91(18)
_cod_database_code               2242855
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.964
_shelx_hkl_checksum              74110
_shelx_res_checksum              62426
_shelxl_version_number           2014/6
_cod_database_fobs_code 2242855