All-inorganic ferric wheel based on hexaniobate-anion linkers
Baranov, Mark; Polin, Libi; Leffler, Nitai; Leitus, Gregory; Shames, Alexander I.; Weinstock, Ira A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00971D

data_7710154
_publ_section_title
;
 All-inorganic ferric wheel based on hexaniobate-anion linkers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00971D
_journal_year                    2022
_chemical_formula_moiety
'Fe8 Li18 Nb48 O162, 52(O), Li8 O2, 1.571(Li14)'
_chemical_formula_sum            'Fe8 Li48 Nb48 O216'
_chemical_formula_weight         8695.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_audit_creation_date             2021-04-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-05 deposited with the CCDC.	2022-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5729(6)
_cell_length_b                   32.4190(3)
_cell_length_c                   43.4373(5)
_cell_measurement_reflns_used    35767
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4080
_cell_measurement_theta_min      4.0960
_cell_volume                     31787.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     19.00 130.00   0.30   10.00    --   45.10  57.00 150.00  370
  2  \w      5.00 118.10   0.30   10.00    --   45.10  57.00   0.00  377
  3  \w     33.00 128.10   0.30   10.00    --   45.10  57.00  60.00  317
  4  \w     -1.00  30.20   0.30   10.00    --   45.10 -77.00-120.00  104
  5  \w     57.00  85.20   0.30   10.00    --   45.10 -77.00-120.00   94
  6  \w     99.00 133.20   0.30   60.00    --  114.00 -77.00  30.00  114
  7  \w     54.00 119.10   0.30   60.00    --  114.00 -77.00-120.00  217
  8  \w     25.00 157.00   0.30   60.00    --  114.00 -77.00   0.00  440
  9  \w     80.00 107.00   0.30   60.00    --  114.00 -77.00 -60.00   90
 10  \w     25.00 127.00   0.30   60.00    --  114.00 -50.00 120.00  340
 11  \w     33.00  75.00   0.30   60.00    --  114.00 -77.00  30.00  140
 12  \w     38.00 123.20   0.30   60.00    --  114.00 -38.00 120.00  284
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0496558000
_diffrn_orient_matrix_UB_12      0.0296620000
_diffrn_orient_matrix_UB_13      0.0100069000
_diffrn_orient_matrix_UB_21      -0.0451900000
_diffrn_orient_matrix_UB_22      0.0355757000
_diffrn_orient_matrix_UB_23      0.0017573000
_diffrn_orient_matrix_UB_31      -0.0122604000
_diffrn_orient_matrix_UB_32      -0.0106201000
_diffrn_orient_matrix_UB_33      0.0339782000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            128352
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.503
_diffrn_reflns_theta_min         3.508
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.118
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       plate
_exptl_crystal_F_000             16192
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.574
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.053
_platon_squeeze_details
;
TITL shelx            P c c n      R = 0.09
CELL   22.5729   32.4190   43.4373     90.00     90.00     90.00
SPGR Pccn
C101 0.352 0.805 0.072 !       4.39 eA-3
C102 0.930 0.572 0.090 !       3.57 eA-3
Q103 0.929 0.990 0.294 !       3.41 eA-3
Q104 0.102 0.846 0.046 !       3.35 eA-3
C105 0.123 0.884 0.326 !       2.98 eA-3
Q106 0.290 0.284 0.794 !       2.92 eA-3
Q107 0.714 0.291 0.257 !       2.92 eA-3
Q108 0.024 0.350 0.598 !       2.83 eA-3
Q109 0.718 0.572 0.480 !       2.81 eA-3
Q110 0.021 0.007 0.171 !       2.78 eA-3
Q111 0.155 0.562 0.183 !       2.76 eA-3
Q112 0.413 0.833 0.270 !       2.64 eA-3
C113 0.141 0.470 0.120 !       2.57 eA-3
Q114 0.118 0.954 0.139 !       2.52 eA-3
Q115 0.401 0.531 0.389 !       2.49 eA-3
Q116 0.734 0.696 0.428 !       2.42 eA-3
Q117 0.194 0.991 0.301 !       2.42 eA-3
Q118 0.580 0.525 0.285 !       2.35 eA-3
Q119 0.357 0.694 0.175 !       2.30 eA-3
Q120 0.177 0.242 0.115 !       2.29 eA-3
Q121 0.250 0.254 0.406 !       2.24 eA-3
C122 0.399 0.876 0.002 !       2.21 eA-3
Q123 0.093 0.591 0.247 !       2.20 eA-3
Q124 0.556 0.367 0.147 !       2.19 eA-3
Q125 0.460 0.204 0.277 !       2.16 eA-3
Q126 0.563 0.328 0.069 !       2.14 eA-3
Q127 0.147 0.073 0.024 !       2.10 eA-3
C128 0.445 0.584 0.448 !       2.09 eA-3
Q129 0.405 0.039 0.154 !       2.06 eA-3
C130 0.113 0.654 0.942 !       2.05 eA-3
Q131 0.744 0.368 0.123 !       2.04 eA-3
C132 0.633 0.578 0.431 !       1.93 eA-3
Q133 0.130 0.092 0.582 !       1.88 eA-3
Q134 0.992 0.679 0.833 !       1.87 eA-3
Q135 0.687 0.779 0.169 !       1.86 eA-3
C136 0.314 0.700 0.097 !       1.86 eA-3
Q137 0.538 0.233 0.168 !       1.82 eA-3
Q138 0.837 0.385 0.539 !       1.79 eA-3
C139 0.774 0.032 0.392 !       1.79 eA-3
Q140 0.229 0.256 0.285 !       1.76 eA-3
Q141 0.624 0.969 0.757 !       1.75 eA-3
Q142 0.976 0.094 0.014 !       1.74 eA-3
Q143 0.485 0.054 0.139 !       1.71 eA-3
Q144 0.541 0.446 0.325 !       1.64 eA-3
Q145 0.305 0.995 0.031 !       1.63 eA-3
Q146 0.698 0.633 0.442 !       1.60 eA-3
C147 0.220 0.897 0.486 !       1.60 eA-3
Q148 0.704 0.092 0.029 !       1.59 eA-3
Q149 0.609 0.302 0.906 !       1.58 eA-3
Q150 0.617 0.790 0.208 !       1.57 eA-3
Q151 0.495 0.665 0.153 !       1.55 eA-3
Q152 0.209 0.704 0.522 !       1.54 eA-3
Q153 0.165 0.625 0.443 !       1.52 eA-3
Q154 0.361 0.319 0.877 !       1.51 eA-3
Q155 0.139 0.222 0.286 !       1.49 eA-3
Q156 0.264 0.604 0.255 !       1.47 eA-3
Q157 0.227 0.350 0.045 !       1.45 eA-3
Q158 0.727 0.650 0.455 !       1.45 eA-3
Q159 0.765 0.934 0.903 !       1.45 eA-3
C160 0.706 0.194 0.014 !       1.44 eA-3
Q161 0.475 0.837 0.246 !       1.44 eA-3
Q162 0.066 0.633 0.717 !       1.44 eA-3
Q163 0.990 0.116 0.295 !       1.42 eA-3
C164 0.484 0.945 0.149 !       1.41 eA-3
Q165 0.487 0.765 0.328 !       1.41 eA-3
Q166 0.032 0.678 0.846 !       1.40 eA-3
C167 0.195 0.680 0.509 !       1.40 eA-3
Q168 0.296 0.875 0.139 !       1.40 eA-3
C169 0.827 0.283 0.555 !       1.40 eA-3
Q170 0.080 0.726 0.596 !       1.40 eA-3
Q171 0.678 0.414 0.191 !       1.38 eA-3
C172 0.115 0.704 0.336 !       1.37 eA-3
Q173 0.470 0.478 0.262 !       1.37 eA-3
Q174 0.531 0.030 0.197 !       1.36 eA-3
Q175 0.094 0.289 0.185 !       1.36 eA-3
Q176 0.617 0.643 0.658 !       1.35 eA-3
Q177 0.227 0.922 0.740 !       1.33 eA-3
C178 0.405 0.835 0.878 !       1.33 eA-3
Q179 0.204 0.088 0.495 !       1.33 eA-3
C180 0.501 0.335 0.119 !       1.33 eA-3
Q181 0.499 0.782 0.314 !       1.30 eA-3
Q182 0.416 0.720 0.922 !       1.30 eA-3
C183 0.749 0.115 0.382 !       1.30 eA-3
Q184 0.641 0.171 0.706 !       1.29 eA-3
Q185 0.236 0.446 0.902 !       1.29 eA-3
Q186 0.665 0.492 0.872 !       1.26 eA-3
Q187 0.983 0.721 0.300 !       1.26 eA-3
Q188 0.565 0.454 0.995 !       1.25 eA-3
Q189 0.210 0.290 0.416 !       1.25 eA-3
Q190 0.323 0.299 0.882 !       1.25 eA-3
Q191 0.797 0.771 0.104 !       1.24 eA-3
C192 0.570 0.423 0.427 !       1.23 eA-3
Q193 0.829 0.490 0.728 !       1.23 eA-3
Q194 0.881 0.202 0.392 !       1.23 eA-3
Q195 0.169 0.296 0.493 !       1.22 eA-3
Q196 0.533 0.797 0.295 !       1.22 eA-3
Q197 0.501 0.273 0.119 !       1.21 eA-3
Q198 0.890 0.007 0.544 !       1.19 eA-3
Q199 0.166 0.334 0.857 !       1.19 eA-3
;
_refine_diff_density_max         1.935
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1449
_refine_ls_number_reflns         31875
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1707P)^2^+31.9223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2338
_refine_ls_wR_factor_ref         0.2479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24542
_reflns_number_total             31875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00971d2.cif
_cod_data_source_block           iw2a_sq
_cod_database_code               7710154
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Nb12Fe1O50Li2
_reflns_odcompleteness_completeness 97.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Li24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Li23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O30) = Uanis(Nb23) = Uanis(Nb25)
2. Others
 Sof(Nb3)=Sof(Nb25)=1-FVAR(1)
 Sof(Nb11)=Sof(Nb23)=FVAR(1)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 59.988
_oxdiff_exptl_absorpt_empirical_full_min 0.413