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_7247933
_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         'C12 F18 K8 N10 O12'
_chemical_formula_sum            'C12 F18 K8 N10 O12'
_chemical_formula_weight         1131.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_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                90
_cell_formula_units_Z            4
_cell_length_a                   23.7161(16)
_cell_length_b                   7.1980(7)
_cell_length_c                   20.5953(18)
_cell_measurement_reflns_used    2727
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      3.43
_cell_volume                     3515.8(5)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0736
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20259
_diffrn_reflns_point_group_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_min         1.978
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0903 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.8578.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 984 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         5798
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0728
_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^)+(0.1100P)^2^+11.5328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.2271
_reflns_Friedel_coverage         0.593
_reflns_Friedel_fraction_full    0.654
_reflns_Friedel_fraction_max     0.616
_reflns_number_gt                3453
_reflns_number_total             5798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01210g2.cif
_cod_data_source_block           09302206_0m
_cod_depositor_comments
'Adding full bibliography for 7247932--7247933.cif.'
_cod_database_code               7247933
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Restrained distances
 C12-C11 = C2-C1 = C4-C3 = C8-C7 = C9-C10 = C6-C5
 1.518 with sigma of 0.0001
 K9-K1
 1.321 with sigma of 0.001
 K2-K10
 1.321 with sigma of 0.001
 K12-K7
 1.321 with sigma of 0.001
 K11-K8
 1.321 with sigma of 0.001
 K4-K13
 1.321 with sigma of 0.001
 K3-K14
 1.321 with sigma of 0.001
 K14-K13
 4.463 with sigma of 0.001
 F16A-C11 = F16-C11
 1.32 with sigma of 0.02
 F16A-F17
 1.86 with sigma of 0.02
 F16A-F18
 2.3 with sigma of 0.02
 K2-K1 \\sim K9-K10
 with sigma of 0.001
 K12-K11 \\sim K8-K7
 with sigma of 0.001
2. Uiso/Uaniso restraints and constraints
F11 \\sim F10 \\sim F12 \\sim C7: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
F16A \\sim C11: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
F16 \\sim C11: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C9) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(K9) = Uanis(K1)
Uanis(K10) = Uanis(K2)
Uanis(K11) = Uanis(K8)
Uanis(K12) = Uanis(K7)
Uanis(K4) = Uanis(K13)
Uanis(K3) = Uanis(K14)
3. Others
 Sof(F16A)=1-FVAR(1)
 Sof(F16)=FVAR(1)
 Fixed Sof: K8(0.95) K7(0.95) K4(0.95) K3(0.95) K2(0.95) K1(0.95) K9(0.05)
 K10(0.05) K12(0.05) K11(0.05) K13(0.05) K14(0.05)
;
_shelx_res_checksum              7407
_olex2_submission_special_instructions 'No special instructions were received'