Effect of counter-ion on packing and crystal density of 5,5'-(3,3'-bi[1,2,4-oxadiazole]-5,5'-diyl)bis(1<i>H</i>-tetrazol-1-olate) with five different cations
Giles, Ian D.; DeHope, Alan J.; Zuckerman, Nathaniel B.; Parrish, Damon A.; Pagoria, Philip F.; Acta Crystallographica Section E 74 (2018) 505–513; doi:10.1107/S205698901800364X

data_2242424
_publ_section_title
;
 Effect of counter-ion on packing and crystal density of
 5,5'-(3,3'-bi[1,2,4-oxadiazole]-5,5'-diyl)bis(1<i>H</i>-tetrazol-1-olate)
 with five different cations
;
_journal_coeditor_code           PK2606
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              505
_journal_page_last               513
_journal_paper_doi               10.1107/S205698901800364X
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '2C1 H4 N5 +, C6 N12 O4 2-, 4H2 O1'
_chemical_formula_moiety         '2(C1 H4 N5 +), C6 N12 O4 2-, 4(H2 O1)'
_chemical_formula_sum            'C8 H16 N22 O8'
_chemical_formula_weight         548.355
_chemical_name_systematic
;
Bis(5-amino-1<i>H</i>-tetrazol-4-ium)
5,5'-(3,3'-bi[1,2,4-oxadiazole]-5,5'-diyl)bis(1<i>H</i>-tetrazol-1-olate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 96.2890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.783(2)
_cell_length_b                   12.7081(11)
_cell_length_c                   6.8396(6)
_cell_measurement_reflns_used    5868
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      52.22
_cell_measurement_theta_min      5.91
_cell_volume                     2141.1(3)
_computing_cell_refinement
;
APEX2 (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2014) and XPREP (Bruker, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18508
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.210
_diffrn_reflns_theta_min         0.827
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9941
_exptl_absorpt_correction_T_min  0.9597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0807P)^2^+0.1085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                3489
_reflns_number_total             4274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2606sup1.cif
_cod_data_source_block           4
_cod_database_code               2242424
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              8096
_shelx_res_checksum              84461
_shelxl_version_number           2016/6
_cod_database_fobs_code 2242424