Mechanistic insights into template-driven polyoxovanadate self-assembly: the role of internal and external templates
Repp, Stefan; Junginger, Kim; Sorsche, Dieter; Zorn, Theresa; Poppler, Ann-Christin; Kikukawa, Yuji; Hayashi, Yoshihito; Streb, Carsten; Dalton Transactions  (2023) –; doi:10.1039/D3DT00252G

data_7712389
_publ_section_title
;
 Mechanistic insights into template-driven polyoxovanadate self-assembly:
 the role of internal and external templates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00252G
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C16 H48 Ba O8 S8, 2(Br0.5), O32 V12, 2(C2 H6 O S), C8 H16 N4, 2(C1.5 H4.5 O0.75 S0.65), 0.7(S1)'
_chemical_formula_sum            'C31 H85 Ba Br N4 O43.5 S12 V12'
_chemical_formula_weight         2423.27
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-10 deposited with the CCDC.	2023-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.6360(13)
_cell_length_b                   19.6360(13)
_cell_length_c                   10.9821(11)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.36
_cell_volume                     4234.4(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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            205894
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         1.854
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.566
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1475 before and 0.0677 after correction. The Ratio of minimum to maximum transmission is 0.9052. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 3701 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.494(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         9764
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0308P)^2^+7.7668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                8149
_reflns_number_total             9764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00252g2.cif
_cod_data_source_block           sr21055_0ma_c
_cod_original_cell_volume        4234.4(7)
_cod_original_formula_sum        'C31 H85 Ba Br N4 O43.50 S12 V12'
_cod_database_code               7712389
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O17) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Others
 Fixed Sof: Br1(0.45) Br2(0.05) S5(0.65) O20(0.75) C10(0.75) H10A(0.75)
 H10B(0.75) H10C(0.75) C14(0.75) H14A(0.75) H14B(0.75) H14C(0.75) S7(0.35)
4.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C33(H33A,H33B), C34(H34A,H34B)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,
 H15B,H15C), C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C10(H10A,H10B,H10C), C14(H14A,H14B,
 H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'