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_7712387
_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, O32 V12, Cl, C8 H24 N4, 4(C H3 O0.6 S0.6), 4(C H3 O0.41 S0.41)'
_chemical_formula_sum            'C32 H96 Cl La N4 O44 S12 V12'
_chemical_formula_weight         2411.48
_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                   19.7197(10)
_cell_length_b                   19.7197(10)
_cell_length_c                   10.9727(6)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.78
_cell_volume                     4266.9(4)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0922
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            57952
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.075
_diffrn_reflns_theta_min         1.856
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.147
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1295 before and 0.0893 after correction. The Ratio of minimum to maximum transmission is 0.8748. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4698
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0227P)^2^+7.4265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4416
_reflns_number_total             4698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00252g2.cif
_cod_data_source_block           sr22074_0ma
_cod_original_cell_volume        4266.9(5)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7712387
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5454(8)
 0.4546(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
 S3-O6 \\sim S3A-O6A
 with sigma of 0.02
 S3-C8 \\sim S3A-C8A
 with sigma of 0.02
 C8-C2 \\sim C8A-C2A
 with sigma of 0.04
 S3-C2 \\sim S3A-C2A
 with sigma of 0.02
 O6-C8 \\sim O6A-C8A
 with sigma of 0.04
 O6-C2 \\sim O6A-C2A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(S3) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C2) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(S3A) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C2A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Sof(S3A)=Sof(O6A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=1-FVAR(1)
 Sof(S3)=Sof(O6)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), N2(H2D,H2E)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C8A(H8AA,H8AB,H8AC), C2A(H2AA,H2AB,H2AC)
;
_olex2_submission_special_instructions 'No special instructions were received'