Supramolecular assembly of a hierarchically structured 3D potassium vanadate framework
Greiner, Simon; Anjass, Montaha; Streb, Carsten; CrystEngComm 23 (2021) 3946–3950; doi:10.1039/D1CE00661D

data_7242907
_publ_section_title
;
 Supramolecular assembly of a hierarchically structured 3D potassium
 vanadate framework
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              3946
_journal_page_last               3950
_journal_paper_doi               10.1039/D1CE00661D
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C27 H39 K10 N13.5 O64 V24, 2(Cl)'
_chemical_formula_sum            'C27 H39 Cl2 K10 N13.5 O64 V24'
_chemical_formula_weight         3261.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-05-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-24 deposited with the CCDC.	2021-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6201(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0012(7)
_cell_length_b                   20.1680(8)
_cell_length_c                   38.2835(16)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.31
_cell_volume                     10018.2(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.1410
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            133193
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.395
_diffrn_reflns_theta_min         1.866
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.689
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1471 before and 0.0817 after correction. The Ratio of minimum to maximum transmission is 0.8575. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_description       needle
_exptl_crystal_F_000             6334
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.358
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1293
_refine_ls_number_reflns         20491
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0792
_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^)+(0.0108P)^2^+115.2684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16530
_reflns_number_total             20491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00661d2.cif
_cod_data_source_block           sg20295_0m
_cod_depositor_comments          'Adding full bibliography for 7242907.cif.'
_cod_original_formula_sum        'C27 H39 Cl2 K10 N13.50 O64 V24'
_cod_database_code               7242907
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.605
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C28
 1.45 with sigma of 0.02
 C27-N14
 1.14 with sigma of 0.02
3. Rigid bond restraints
 N5, C15, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C17, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N11, C23, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N9, C21, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N13, C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N7, C24, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, C18, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N12, C13, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N10, C10, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C1, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N14, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N14, C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C9, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N5 \\sim C15 \\sim C12: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N4 \\sim C17 \\sim C20: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N11 \\sim C23 \\sim C22: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N9 \\sim C21 \\sim C14: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N13 \\sim C25 \\sim C26: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N7 \\sim C24 \\sim C19: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N8 \\sim C18 \\sim C11: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N1 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
N12 \\sim C13 \\sim C8: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N3 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
N10 \\sim C10 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N2 \\sim C1 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
N14 \\sim C27: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
N14 \\sim C27 \\sim C28: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N6 \\sim C9 \\sim C7: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
5. Others
 Fixed Sof: N14(0.5) C27(0.5) C28(0.5)
6.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'