Reactivity control of nitrate-incorporating octadecavanadates by changing the oxidation state and metal substitution.
Yoshida, Isshin; Kikukawa, Yuji; Mitsuhashi, Ryoji; Hayashi, Yoshihito; Nanoscale 16 (2024) 10584–10589; doi:10.1039/d4nr01243g

data_1571523
_publ_section_title
;
 Reactivity control of nitrate-incorporating octadecavanadates by changing
 the oxidation state and metal substitution.
;
_journal_issue                   22
_journal_name_full               Nanoscale
_journal_page_first              10584
_journal_page_last               10589
_journal_paper_doi               10.1039/d4nr01243g
_journal_volume                  16
_journal_year                    2024
_chemical_formula_sum            'C54 H121 N8 O49 V18'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    !SHELXS-2013/1'
_diffrn_ambient_temperature      83(2)
_diffrn_detector_area_resol_mean 14.4613
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Mercury (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
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_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48442
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         30.332
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
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_exptl_crystal_density_meas      ?
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_exptl_crystal_size_mid          0.200
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_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 4743 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.030(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         12733
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_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0617P)^2^+4.5985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.825
_reflns_number_gt                11780
_reflns_number_total             12733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nr01243g2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1571523.cif.
;
_cod_original_cell_volume        4828.26(15)
_cod_database_code               1571523
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.722
_shelx_estimated_absorpt_t_max   0.722
_shelx_res_checksum              170