Three-dimensional alkaline earth metal–organic framework poly[[μ-aqua-aquabis(μ3-carbamoylcyanonitrosomethanido)barium] monohydrate] and its thermal decomposition
Domasevitch, Kostiantyn V.; Senchyk, Ganna A.; Ponomarova, Vira V.; Lysenko, Andrey B.; Krautscheid, Harald; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 986–992; doi:10.1107/S2056989024008375

data_2023242
_publ_section_title
;
 Three-dimensional alkaline earth metal--organic framework
 poly[[\m-aqua-aquabis(\m3-carbamoylcyanonitrosomethanido)barium]
 monohydrate] and its thermal decomposition
;
_journal_coeditor_code           YZ2057
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              986
_journal_page_last               992
_journal_paper_doi               10.1107/S2056989024008375
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Ba (C3 H2 N3 O2)2 (H2 O1)2], H2 O'
_chemical_formula_moiety         'C6 H8 Ba N6 O6, H2 O'
_chemical_formula_sum            'C6 H10 Ba N6 O7'
_chemical_formula_weight         415.54
_chemical_name_systematic
;
Poly[[\m-aqua-aquabis(\m~3~-carbamoylcyanonitrosomethanido)barium]
monohydrate]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6667(17)
_cell_length_b                   4.4102(7)
_cell_length_c                   11.2816(14)
_cell_measurement_reflns_used    3251
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.441
_cell_measurement_theta_min      4.622
_cell_volume                     679.97(16)
_computing_cell_refinement
;
X-AREA 1.76 (Stoe & Cie, 2016)
;
_computing_data_collection
;
X-AREA 1.76 (Stoe & Cie, 2016)
;
_computing_data_reduction
;
X-AREA 1.76 (Stoe & Cie, 2016)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX 1.70.01 (Farrugia, 2012)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe Image plate diffraction system-2T'
_diffrn_measurement_method       '\f oscillation scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3251
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.441
_diffrn_reflns_theta_min         4.622
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.962
_exptl_absorpt_correction_T_max  0.3994
_exptl_absorpt_correction_T_min  0.3099
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_description       prism
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.724
_refine_diff_density_min         -1.866
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 668 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.013(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1696
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0169
_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^)+(0.0318P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                1688
_reflns_number_total             1696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2057.cif
_cod_data_source_block           I
_cod_database_code               2023242
_shelx_estimated_absorpt_t_min   0.562
_shelx_estimated_absorpt_t_max   0.665
_shelx_hkl_checksum              13467
_shelx_res_checksum              49779