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_7245242
_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         'C72 H146 N2 Nb8 O40'
_chemical_formula_sum            'C72 H146 N2 Nb8 O40'
_chemical_formula_weight         2423.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-01-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-16 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                68.271(4)
_cell_angle_beta                 81.253(5)
_cell_angle_gamma                84.084(5)
_cell_formula_units_Z            1
_cell_length_a                   8.0483(9)
_cell_length_b                   18.5558(19)
_cell_length_c                   18.624(2)
_cell_measurement_reflns_used    2832
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.37
_cell_volume                     2550.4(5)
_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      100.01
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_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  0.0999
_diffrn_reflns_av_unetI/netI     0.1692
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31082
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         1.339
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0751 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.8913.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.746
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10333
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5345
_reflns_number_total             10333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00828a2.cif
_cod_data_source_block           gar218
_cod_database_code               7245242
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.885
_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
 C21B-C22B
 1.5 with sigma of 0.02
 O10-C21B
 1.4 with sigma of 0.02
 C21A-O10
 1.4 with sigma of 0.02
 C22A-C21A
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C35A, C36A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13A, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13B, C14B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33A, C34A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33B, C34B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C13B) \\sim Ueq, Uanis(C14B) \\sim Ueq, Uanis(C13A) \\sim Ueq,
Uanis(C21B) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C35B) \\sim Ueq,
Uanis(C35A) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.02
Uanis(C24B) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. Others
 Sof(C13B)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=1-FVAR(1)
 Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(2)
 Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=FVAR(2)
 Sof(C36B)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35B)=Sof(H35A)=Sof(H35B)=1-FVAR(3)
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=FVAR(3)
 Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(4)
 Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=FVAR(4)
 Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H22C)=1-FVAR(5)
 Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B), C11(H11A,H11B), C9(H9A,H9B),
 C23(H23A,H23B), C23(H23C,H23D), C33B(H33A,H33B), C29(H29A,H29B), C31(H31A,
 H31B), C35B(H35A,H35B), C13B(H13A,H13B), C27(H27A,H27B), C25(H25A,H25B),
 C13A(H13C,H13D), C21B(H21A,H21B), C35A(H35C,H35D), C33A(H33C,H33D), C21A(H21C,
 H21D)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C12(H12A,H12B,
 H12C), C10(H10A,H10B,H10C), C36B(H36A,H36B,H36C), C26(H26A,H26B,H26C),
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C34A(H34A,H34B,H34C), C14A(H14A,H14B,
 H14C), C24A(H24A,H24B,H24C), C14B(H14D,H14E,H14F), C22B(H22A,H22B,H22C),
 C24B(H24D,H24E,H24F), C36A(H36D,H36E,H36F), C34B(H34D,H34E,H34F), C28(H28A,
 H28B,H28C), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              17405
_shelx_hkl_checksum              91522
_olex2_submission_special_instructions 'No special instructions were received'