Temperature-induced pseudopolymorphism of molecular salts from a pyridyl bis-urea macrocycle and naphthalene-1,5-disulfonic acid
Som, Bozumeh; Shue, Jessica R.; Smith, Mark D.; Shimizu, Linda S.; Acta Crystallographica Section C 74 (2018) 75–81; doi:10.1107/S2053229617017600

data_2020989
_publ_section_title
;
 Temperature-induced pseudopolymorphism of molecular salts from a pyridyl
 bis-urea macrocycle and naphthalene-1,5-disulfonic acid
;
_journal_coeditor_code           FN3249
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              75
_journal_page_last               81
_journal_paper_doi               10.1107/S2053229617017600
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'C16 H20 N6 O2 2+, C10 H6 O6 S2 2-, C2 H6 O S'
_chemical_formula_moiety
'C16 H20 N6 O2 2+, C10 H6 O6 S2 2-, C2 H6 O S'
_chemical_formula_sum            'C28 H32 N6 O9 S3'
_chemical_formula_weight         692.77
_chemical_name_systematic
;4,14-Dioxo-3,5,13,15,21,22-hexaazatricyclo[15.3.1.1^7,11^]docosa-1(21),7(22),8,10,17,19-hexaene-21,22-diium naphthalene-1,5-disulfonate dimethyl sulfoxide
monosolvate
;
_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   mixed
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;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
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_cell_length_c                   13.6411(6)
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_cell_measurement_temperature    200(2)
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;
SAINT (Bruker, 2015)
;
_computing_data_collection
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APEX2 (Bruker, 2016)
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SAINT (Bruker, 2015)
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<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
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<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
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SHELXL2014 (Sheldrick, 2015b)
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;
SHELXT (Sheldrick, 2015a)
;
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_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52398
_diffrn_reflns_theta_full        27.158
_diffrn_reflns_theta_max         27.158
_diffrn_reflns_theta_min         2.222
_diffrn_standards_number         0
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;
(SADABS; Bruker, 2016)
;
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_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.377
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_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.029
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0310P)^2^+2.4238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                5142
_reflns_number_total             6634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3249sup1.cif
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_cod_database_code               2020989
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.957
_shelx_hkl_checksum              47089
_shelx_res_checksum              81130
_cod_database_fobs_code 2020989