Molecular niobium(V) complexes with mononuclear {Nb1} and dinuclear oxo species {Nb2O} connected through aryl di- or tetra-carboxylate linker
Andriotou, Despoina; Duval, Sylvain; Trivelli, Xavier; Volkringer, Christophe; Loiseau, Thierry; CrystEngComm  (2022) –; doi:10.1039/D2CE00828A

data_7245241
_publ_section_title
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 Molecular niobium(V) complexes with mononuclear {Nb1} and dinuclear oxo
 species {Nb2O} connected through aryl di- or tetra-carboxylate linker
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00828A
_journal_year                    2022
_chemical_formula_moiety         'C58 H122 Nb6 O34'
_chemical_formula_sum            'C58 H122 Nb6 O34'
_chemical_formula_weight         1921.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-22
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2022-06-16 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.312(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0297(14)
_cell_length_b                   18.1938(11)
_cell_length_c                   19.0238(11)
_cell_measurement_reflns_used    9438
_cell_measurement_temperature    106.73
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.67
_cell_volume                     8249.4(8)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      106.73
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.972
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62529
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_min         1.707
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1606 before and 0.0496 after correction.
The Ratio of minimum to maximum transmission is 0.8237.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.45
_refine_diff_density_max         2.278
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         8239
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0598P)^2^+92.2868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6659
_reflns_number_total             8239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00828a2.cif
_cod_data_source_block           da770
_cod_database_code               7245241
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.520
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22A-C23A
 1.45 with sigma of 0.02
 C20B-C21B
 1.45 with sigma of 0.02
 C20A-C21A
 1.45 with sigma of 0.02
 C29B-C28B
 1.45 with sigma of 0.02
 C2-C1
 1.45 with sigma of 0.02
3. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20B, C21B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20B \\sim C21B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C28B \\sim C29B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C23B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C22B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C20A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
5. Others
 Sof(O11B)=Sof(C19B)=Sof(O12B)=Sof(Nb3B)=Sof(O13B)=Sof(O17B)=Sof(O15B)=
 Sof(O14B)=Sof(O16B)=Sof(C28B)=Sof(H28A)=Sof(H28B)=Sof(C23B)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H24C)=Sof(H24D)=
 Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(C27B)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(O12A)=Sof(Nb3A)=Sof(C19A)=Sof(O11A)=Sof(O17A)=
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=
 Sof(O16A)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(O15A)=Sof(O14A)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(O13A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C5(H5A,H5B), C13(H13A,H13B), C3(H3A,H3B), C11(H11A,
 H11B), C1(H1A,H1B), C28B(H28A,H28B), C22B(H22A,H22B), C24(H24C,H24D), C24(H24A,
 H24B), C20B(H20A,H20B), C26B(H26A,H26B), C26A(H26C,H26D), C28A(H28C,H28D),
 C22A(H22C,H22D), C20A(H20C,H20D)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C6(H6A,H6B,
 H6C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C23B(H23A,H23B,H23C),
 C25(H25A,H25B,H25C), C27B(H27A,H27B,H27C), C27A(H27D,H27E,H27F), C29A(H29A,
 H29B,H29C), C23A(H23D,H23E,H23F), C21A(H21A,H21B,H21C), C29B(H29D,H29E,H29F),
 C21B(H21D,H21E,H21F)
;
_shelx_res_checksum              70910
_shelx_hkl_checksum              31803
_olex2_submission_special_instructions 'No special instructions were received'