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_7712388
_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_formula_moiety
'C16 H48 La O8 S8, 4(Br0.25), O32 V12, C8 H24 N4, 4(C2 H6 O S)'
_chemical_formula_sum            'C32 H96 Br La N4 O44 S12 V12'
_chemical_formula_weight         2455.94
_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
_audit_creation_date             2022-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-22 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                   19.7295(7)
_cell_length_b                   19.7295(7)
_cell_length_c                   10.9901(5)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.36
_cell_volume                     4277.9(3)
_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)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0767
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33977
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         3.459
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1691 before and 0.0786 after correction. The Ratio of minimum to maximum transmission is 0.7903. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       plate
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.549
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0929P)^2^+6.4376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3862
_reflns_number_total             4057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00252g2.cif
_cod_data_source_block           sr22159_0ma
_cod_original_cell_volume        4277.9(4)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7712388
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5974(17)
 0.4026(17)
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. Rigid bond restraints
 S3, O1, S2, C2, C1, C5, H1A, H1B, H1C, H5A, H5B, H5C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
S3 \\sim O1 \\sim S2 \\sim C2 \\sim C1 \\sim C5 \\sim H1A \\sim H1B \\sim H1C
\\sim H5A \\sim H5B \\sim H5C: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(S3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, : with sigma of 0.1 and sigma
for terminal atoms of 0.2
5. Others
 Fixed Sof: Br02(0.23875) S2(0.45) S3(0.55) C1(0.45) H1A(0.45) H1B(0.45)
 H1C(0.45) C5(0.55) H5A(0.55) H5B(0.55) H5C(0.55) Br1(0.01125)
6.a Secondary CH2 refined with riding coordinates:
 N00K(H00D,H00E), C00M(H00F,H00G), C00U(H00H,H00I)
6.b Idealised Me refined as rotating group:
 C00W(H00A,H00B,H00C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C),
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'