Crystal structure of tetrakis(1-oxidopyridin-2-yl)methane methanol tetrasolvate
Matsumoto, Kouzou; Kawashita, Kazuaki; Kannami, Masaki; Oda, Masaji; Acta Crystallographica Section E 71 (2015) o754–o755; doi:10.1107/S2056989015016862

data_2241108
_publ_section_title
;
 Crystal structure of tetrakis(1-oxidopyridin-2-yl)methane methanol
 tetrasolvate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o754
_journal_page_last               o755
_journal_paper_doi               10.1107/S2056989015016862
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C21 H16 N4 O4, 4C H4 O'
_chemical_formula_moiety         'C21 H16 N4 O4, 4(C H4 O)'
_chemical_formula_sum            'C25 H32 N4 O8'
_chemical_formula_weight         516.54
_chemical_name_common
'Tetrakis(pyridin-2-yl)methane tetra<i>N</i>-oxide methanol tetrasolvate'
_chemical_name_systematic
;
Tetrakis(1-oxidopyridin-2-yl)methane methanol tetrasolvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4474(4)
_cell_length_b                   14.4474(4)
_cell_length_c                   12.2965(5)
_cell_measurement_reflns_used    9662
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.6
_cell_volume                     2566.62(14)
_computing_cell_refinement
;
<i>PROCESS-AUTO</i> (Rigaku, 1998)
;
_computing_data_collection
;
<i>PROCESS-AUTO</i> (Rigaku, 1998)
;
_computing_data_reduction
;
<i>PROCESS-AUTO</i> (Rigaku, 1998)
;
_computing_molecular_graphics
;
<i>Yadokari-XG 2009</i> (Wakita, 2001) and
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
<i>Yadokari-XG 2009</i> (Wakita, 2001) and
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12321
_diffrn_reflns_theta_full        25.2
_diffrn_reflns_theta_max         27.4
_diffrn_reflns_theta_min         3.6
_exptl_absorpt_coefficient_mu    0.10
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.053
_refine_ls_R_factor_gt           0.049
_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^)+(0.0821P)^2^+1.7364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.134
_refine_ls_wR_factor_ref         0.138
_reflns_number_gt                1289
_reflns_number_total             1470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5417sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2566.62(18)
_cod_database_code               2241108
_cod_database_fobs_code          2241108
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.990
_shelx_hkl_checksum              91335
_shelx_res_checksum              60691