Regulation of the structure and density of KN5 frameworks with CH3COOK and CF3COOK
Jiang, Shuaijie; Zhou, Jianxin; Xu, Yuangang; Lin, Qiuhan; Wang, Pengcheng; Lu, Ming; CrystEngComm 26 (2024) 951–956; doi:10.1039/D3CE01210G

data_7247932
_publ_section_title
;
 Regulation of the structure and density of KN5 frameworks with CH3COOK
 and CF3COOK
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              951
_journal_page_last               956
_journal_paper_doi               10.1039/D3CE01210G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C6 H9 K5 N10 O6'
_chemical_formula_sum            'C6 H9 K5 N10 O6'
_chemical_formula_weight         512.73
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-09-19 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   10.3592(2)
_cell_length_b                   10.3592(2)
_cell_length_c                   20.7675(8)
_cell_measurement_reflns_used    3671
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      3.00
_cell_volume                     1930.04(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      243.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         2.270
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0732 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.8836.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1152
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0250P)^2^+0.9464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                985
_reflns_number_total             1152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01210g2.cif
_cod_data_source_block           mo_0920_0m
_cod_depositor_comments
'Adding full bibliography for 7247932--7247933.cif.'
_cod_original_cell_volume        1930.04(11)
_cod_database_code               7247932
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.861
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5-N8 = N8-N9
 1.3 with sigma of 0.02
 N8-N9 = N9-N6
 1.3 with sigma of 0.02
 N9-N6 = N6-N4
 1.3 with sigma of 0.02
 N4-N5 = N5-N8
 1.3 with sigma of 0.02
 K003-N5
 2.934 with sigma of 0.001
 N8-N6
 2.117 with sigma of 0.04
 N4-N8
 2.117 with sigma of 0.04
 N9-N4
 2.117 with sigma of 0.04
 N5-N9
 2.117 with sigma of 0.04
3. Restrained planarity
 N5, N4, N6, N8, N9
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N8) \\sim
Ueq, Uanis(N9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Rigid body (RIGU) restrains
 N008, N009, N1, N2, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N5, N4, N6, N8, N9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: N009(0.5) N008(0.5) N1(0.5) N3(0.5) N2(0.5) N5(0.16667)
 N4(0.16667) N6(0.16667) N8(0.16667) N9(0.16667)
7.a Idealised Me refined as rotating group:
 C007(H00A,H00B,H00C)
;
_shelx_res_checksum              53091
_olex2_submission_special_instructions 'No special instructions were received'