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_7245243
_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         'C42 H78 N2 Nb4 O20'
_chemical_formula_sum            'C42 H78 N2 Nb4 O20'
_chemical_formula_weight         1302.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-15
_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                 90.114(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3902(12)
_cell_length_b                   20.0542(14)
_cell_length_c                   17.5280(13)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.32
_cell_volume                     5409.8(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0479
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         1.323
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1030 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.9382.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11078
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0353P)^2^+6.2184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10247
_reflns_number_total             11078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00828a2.cif
_cod_data_source_block           gar217monop
_cod_database_code               7245243
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.813
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6793(6)
 0.3207(6)
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
3. Restrained distances
 C27A-C26A
 1.45 with sigma of 0.02
 C26B-C27B
 1.45 with sigma of 0.02
 C32-C33
 1.5 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C14B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C27A) = Uanis(C26A) = Uanis(C26B) = Uanis(C27B)
5. Others
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(1)
 Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=FVAR(1)
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C14B)=Sof(H14C)=Sof(H14D)=1-FVAR(2)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C38(H38A,H38B), C30(H30A,H30B), C22(H22A,H22B), C40(H40A,
 H40B), C24(H24A,H24B), C32(H32A,H32B), C20(H20A,H20B), C16(H16A,H16B),
 C14A(H14A,H14B), C34(H34A,H34B), C28(H28A,H28B), C36(H36A,H36B), C14B(H14C,
 H14D), C26B(H26A,H26B), C26A(H26C,H26D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C11(H11), C4(H4), C13(H13), C9(H9), C10(H10)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C21(H21A,
 H21B,H21C), C17(H17A,H17B,H17C), C15A(H15A,H15B,H15C), C35(H35A,H35B,H35C),
 C37(H37A,H37B,H37C), C29(H29A,H29B,H29C), C15B(H15D,H15E,H15F), C27A(H27A,H27B,
 H27C), C27B(H27D,H27E,H27F)
;
_shelx_res_checksum              20416
_shelx_hkl_checksum              43033
_olex2_submission_special_instructions 'No special instructions were received'