Cation-controlled capture of polyoxovanadate-based organic-inorganic 1D architectures
Repp, Stefan; Steiner, Michael; Anjass, Montaha; Sorsche, Dieter; Streb, Carsten; Chemical Communications  (2022) –; doi:10.1039/D2CC04379C

data_7130978
_publ_section_title
;
 Cation-controlled capture of polyoxovanadate-based organic-inorganic 1D
 architectures
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04379C
_journal_year                    2022
_chemical_formula_moiety
'C16 H48 Ba O8 S8, O32 V12, N O3, C8 H24 N4, 4(C2 H6 O S)'
_chemical_formula_sum            'C32 H96 Ba N5 O47 S12 V12'
_chemical_formula_weight         2436.47
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-08-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6214)
;
_audit_update_record
;
2022-08-02 deposited with the CCDC.	2022-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6114(12)
_cell_length_b                   19.6114(12)
_cell_length_c                   11.0115(9)
_cell_measurement_reflns_used    9486
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.36
_cell_volume                     4235.1(5)
_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 2014/7 (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 1.000
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            368824
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_min         1.849
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6595
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1188 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.8845.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       block
_exptl_crystal_F_000             2446
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0358P)^2^+5.9095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4793
_reflns_number_total             4893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04379c2.cif
_cod_data_source_block           sr21028_0ma
_cod_original_cell_volume        4235.1(6)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7130978
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5000(8)
 0.5000(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S2-O1 \\sim S2A-O1A
 with sigma of 0.02
 S2-C1 \\sim S2A-C1A
 with sigma of 0.02
 S2-C3 \\sim S2A-C3A
 with sigma of 0.02
 O1-C3 \\sim O1A-C3A
 with sigma of 0.04
 O1-C1 \\sim O1A-C1A
 with sigma of 0.04
 C1-C3 \\sim C1A-C3A
 with sigma of 0.04
4. Rigid body (RIGU) restrains
 S2, O1, C1, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2A, O1A, C1A, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S2A)=Sof(O1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(S2)=Sof(O1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=FVAR(1)
 Fixed Sof: O5(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), N5(H5D,H5E), C8(H8A,H8B)
6.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C1A(H1AA,H1AB,H1AC), C3A(H3AA,H3AB,H3AC)
;
_olex2_submission_special_instructions 'No special instructions were received'