Formation of a meltable purinate metal-organic framework and its glass analogue.
Bumstead, Alice M.; Castillo-Blas, Celia; Pakamorė, Ignas; Thorne, Michael F.; Sapnik, Adam F.; Chester, Ashleigh M.; Robertson, Georgina; Irving, Daniel J. M.; Chater, Philip A.; Keen, David A.; Forgan, Ross S.; Bennett, Thomas D.; Chemical communications (Cambridge, England) 59 (2023) 732–735; doi:10.1039/d2cc05314d

data_7131079
_publ_section_title
;
 Formation of a meltable purinate metal-organic framework and its glass
 analogue.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              732
_journal_page_last               735
_journal_paper_doi               10.1039/d2cc05314d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C13 H12 N9 Zn2'
_chemical_formula_sum            'C13 H12 N9 Zn2'
_chemical_formula_weight         425.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-27 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.1336(5)
_cell_length_b                   15.4532(5)
_cell_length_c                   18.4151(6)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.692
_cell_volume                     4306.6(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36647
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.317
_diffrn_reflns_theta_min         2.692
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.239
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1153 before and 0.0621 after correction. The Ratio of minimum to maximum transmission is 0.6566. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       Squere
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5181
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0363P)^2^+5.7793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4155
_reflns_number_total             5181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05314d2.cif
_cod_data_source_block           mo_uc220322_150k_0m_sq
_cod_depositor_comments          'Adding full bibliography for 7131079.cif.'
_cod_database_code               7131079
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.534
_shelx_estimated_absorpt_t_min   0.337
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C11-C12
 1.4 with sigma of 0.02
 C13A-C11
 1.434 with sigma of 0.02
 N9A-C13A
 1.407 with sigma of 0.02
 N10A-C12
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim N3 \\sim C1 \\sim N4: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
N4 \\sim C1 \\sim N3 \\sim C3A \\sim C2A: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
N10 \\sim C13 \\sim N9 \\sim C14 \\sim C12 \\sim C11 \\sim N7 \\sim N8 \\sim
C10: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C14A \\sim N9A \\sim C13A \\sim C11 \\sim C12 \\sim N10A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: H12(0.5) H11(0.5) C3A(0.5) H3A(0.5) C2A(0.5) H2A(0.5) N9(0.375)
 N10(0.375) C14(0.375) H14(0.375) C13(0.375) H13(0.375) C2(0.5) H2(0.5) C3(0.5)
 H3(0.5) N10A(0.125) C14A(0.125) H14A(0.125) N9A(0.125) C13A(0.125) H13A(0.125)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C9(H9), C12(H12), C1(H1), C11(H11), C8(H8), C6(H6), C5(H5),
 C7(H7), C3A(H3A), C2A(H2A), C14(H14), C13(H13), C2(H2), C3(H3), C14A(H14A),
 C13A(H13A)
;
_shelx_res_checksum              24759
_shelx_hkl_checksum              4370
_shelx_fab_checksum              9684
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'