A NbO-type mixed lanthanide metal-organic framework for cryogenic temperature sensing.
Li, Yi; Zhang, Xiaoman; Wang, Huizhen; Zhang, Lin; Li, Hongjun; Zhao, Dian; Chemical communications (Cambridge, England) 61 (2024) 342–345; doi:10.1039/d4cc04715j

data_7134013
_publ_section_title
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 A NbO-type mixed lanthanide metal-organic framework for cryogenic
 temperature sensing.
;
_journal_issue                   2
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              342
_journal_page_last               345
_journal_paper_doi               10.1039/d4cc04715j
_journal_volume                  61
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C159 H157 N22 O89 Tb12, 7[C3H7NO], 7[C3H7NO], 7[C3H7NO], 1.333[]'
_chemical_formula_sum            'C222 H298 N43 O110 Tb12'
_chemical_formula_weight         7236.169
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_Int_Tables_number      154
_audit_creation_date             2024-09-17
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.09.12 svn.r2332d2e9 for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-11-01 deposited with the CCDC.	2024-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   19.9247(18)
_cell_length_b                   19.9247(18)
_cell_length_c                   68.595(9)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    247(2)
_cell_measurement_theta_max      28.6835
_cell_measurement_theta_min      2.9215
_cell_volume                     23583(4)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_reduction        'SAINT V8.40B'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS (G. Sheldrick)'
_diffrn_ambient_temperature      247.15
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9974
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Ius Duo PHOTON II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.9972
_diffrn_reflns_Laue_measured_fraction_max 0.9974
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       93
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            169615
_diffrn_reflns_point_group_measured_fraction_full 0.9978
_diffrn_reflns_point_group_measured_fraction_max 0.9980
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    2.747
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             10782.004
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details          )
_refine_diff_density_max         1.6845
_refine_diff_density_min         -2.3300
_refine_diff_density_rms         0.1742
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.303(4)
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             9.5669
_refine_ls_goodness_of_fit_ref   1.0290
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    158
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         30883
_refine_ls_number_restraints     1963
_refine_ls_restrained_S_all      0.9964
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+174.2824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.999
_reflns_limit_h_max              21
_reflns_limit_h_min              -20
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              84
_reflns_limit_l_min              -84
_reflns_number_gt                29056
_reflns_number_total             30883
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc04715j2.cif
_cod_data_source_block           NbO-TbPDDI
_cod_depositor_comments          'Adding full bibliography for 7134013.cif.'
_cod_original_sg_symbol_Hall     ' P 32 2"'
_cod_database_code               7134013
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.819(8)
 0.181(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups, All O(H,H,H,H) groups
3. Restrained distances
 C21_2-C18_2
 1.53 with sigma of 0.01
 N1_11-O1_11 \\sim N1_11-O2_11 \\sim N1_11-O3_11
 with sigma of 0.02
 O1_11-O2_11 \\sim O2_11-O3_11 \\sim O3_11-O1_11
 with sigma of 0.04
 N1_5-C2_5 \\sim N1_5-C3_5
 N1_6-C2_6 \\sim N1_6-C3_6
 N1_7-C2_7 \\sim N1_7-C3_7
 N1_8-C2_8 \\sim N1_8-C3_8
 N1_10-C2_10 \\sim N1_10-C3_10
 N1_12-C2_12 \\sim N1_12-C3_12
 with sigma of 0.02
 N1_5-C1_5
 N1_6-C1_6
 N1_7-C1_7
 N1_8-C1_8
 N1_10-C1_10
 N1_12-C1_12
 with sigma of 0.02
 C1_5-O1_5
 C1_6-O1_6
 C1_7-O1_7
 C1_8-O1_8
 C1_10-O1_10
 C1_12-O1_12
 with sigma of 0.02
 C2_5-C3_5
 C2_6-C3_6
 C2_7-C3_7
 C2_8-C3_8
 C2_10-C3_10
 C2_12-C3_12
 with sigma of 0.04
 C1_5-C3_5
 C1_6-C3_6
 C1_7-C3_7
 C1_8-C3_8
 C1_10-C3_10
 C1_12-C3_12
 with sigma of 0.04
 C1_5-C2_5
 C1_6-C2_6
 C1_7-C2_7
 C1_8-C2_8
 C1_10-C2_10
 C1_12-C2_12
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O1_10) \\sim Ueq, Uanis(O1A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O11) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O6)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
5. Same fragment restrains
{C9_2, N1A_2, C11A_2, C12_2, C13A_2, C10A_2} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C9_2, N1_2, C11_2, C12_2, C13_2, C10_2}
{C9_1, N1A_1, C11A_1, C12_1, C10A_1, C13A_1} sigma for 1-2: 0.01, 1-3: 0.04
as in
{C9_1, N1_1, C11_1, C12_1, C10_1, C13_1}
{C1_6, O1_6, N1_6, C2_6, C3_6}
{C1_7, O1_7, N1_7, C2_7, C3_7}
{C1_8, O1_8, N1_8, C2_8, C3_8}
{C1_10, O1_10, N1_10, C2_10, C3_10}
{C1_12, O1_12, N1_12, C2_12, C3_12}
as
{C1_5, O1_5, N1_5, C2_5, C3_5} sigma for 1-2: 0.02 1-3: 0.04
6. Others
 Sof(N1A)=Sof(C11A)=Sof(H11A)=Sof(C10A)=Sof(H10A)=Sof(C13A)=Sof(H13A)=1-FVAR(1)
 Sof(N1)=Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=Sof(C13)=Sof(H13)=FVAR(1)
 Sof(N1A)=Sof(C11A)=Sof(H11A)=Sof(C13A)=Sof(H13A)=Sof(C10A)=Sof(H10A)=1-FVAR(2)
 Sof(N1)=Sof(C11)=Sof(H11)=Sof(C13)=Sof(H13)=Sof(C10)=Sof(H10)=FVAR(2)
 Fixed Sof: O7(0.5) O1A(0.5) H1Aa(0.5) H7a(0.5) H7b(0.5) H1Ab(0.5) O8(0.5)
 H8a(0.5) H8b(0.5) O9(0.5) O6(0.5) H6a(0.5) H6b(0.5) O11(0.5) H11a(0.5)
 H11b(0.5) O12(0.5) H12a(0.5) H12b(0.5) C10X(0.5) H10X(0.5) C10Y(0.5) H10Y(0.5)
 N1X(0.5) C11X(0.5) H11X(0.5) N1X(0.5) C10X(0.5) H10X(0.5) C11X(0.5) H11X(0.5)
 C10Y(0.5) H10Y(0.5) C1(0.5) H1(0.5) O1(0.5) N1(0.5) C2(0.5) H2a(0.5) H2b(0.5)
 H2c(0.5) C3(0.5) H3a(0.5) H3b(0.5) H3c(0.5) N1(0.5) O1(0.5) O2(0.5) O3(0.5)
7.a Riding coordinates:
 O5(O15,H5a,H5b,H15a,H15b,O13,H13a,H13b), O1(H1a,H1b,O7,O1A,H1Aa,H7a,H7b,H1Ab,
 O8,H8a,H8b), O6(H6a,H6b,O11,H11a,H11b,O12,H12a,H12b), C10X(H10X), C10Y(H10Y)
7.b Me refined with riding coordinates:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C2(H2a,
 H2b,H2c), C3(H3a,H3b,H3c), C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C2(H2a,H2b,H2c),
 C3(H3a,H3b,H3c), C3(H3a,H3b,H3c)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11), C10(H10), C13(H13), C11A(H11A), C10A(H10A),
 C13A(H13A), C15(H15), C17(H17), C19(H19), C3(H3), C5(H5), C7(H7), C11(H11),
 C13(H13), C10(H10), C11A(H11A), C13A(H13A), C10A(H10A), C15(H15), C17(H17),
 C19(H19), C3(H3), C5(H5), C7(H7), C10Y(H10Y), C11X(H11X), C7(H7), C5(H5),
 C3(H3), C10X(H10X), C11X(H11X), C1(H1), C1(H1), C1(H1), C1(H1), C1(H1), C1(H1)
7.d Fitted hexagon refined as free rotating group:
 C9(N1,C11,C12,C10,C13), C9(N1,C11,C12,C13,C10)
7.e X=CH2 refined with riding coordinates:
 C2(H2a,H2b)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_special_details
;
A solvent mask was calculated and 2571 electrons were
found in a volume of 9755\%A^3^ in 4 voids per unit cell.
This is consistent with the presence of  7[C3H7NO], 7[C3H7NO], 7[C3H7NO] 
per Formula Unit  which account for 2520 electrons  per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_olex2_submission_special_instructions 'No special instructions were received'