Two synthetic routes generate two isopolyoxoniobates based on {Nb16} and {Nb20}
Niu, Jingyang; Liang, Zhijie; Qiao, Yuanyuan; Li, Miaomiao; Ma, Pengtao; Wang, Jingping; Dalton Transactions  (2019) –; doi:10.1039/C9DT04147H

data_7701995
_publ_section_title
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 Two synthetic routes generate two isopolyoxoniobates based on {Nb16} and
 {Nb20}
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04147H
_journal_year                    2019
_chemical_formula_moiety         'C110 H106 Cu11 N22 Nb20 O70, 61(H2O)'
_chemical_formula_sum            'C110 H228 Cu11 N22 Nb20 O131'
_chemical_formula_weight         6512.27
_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     dual
_audit_creation_date             2019-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-18 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                97.782(2)
_cell_angle_beta                 94.0890(10)
_cell_angle_gamma                115.1800(10)
_cell_formula_units_Z            2
_cell_length_a                   19.1459(7)
_cell_length_b                   19.6390(8)
_cell_length_c                   35.0769(15)
_cell_measurement_reflns_used    9109
_cell_measurement_temperature    296
_cell_measurement_theta_max      29.433
_cell_measurement_theta_min      2.332
_cell_volume                     11703.1(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            128012
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         2.136
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    2.011
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1001 before and 0.0503 after correction. The Ratio of minimum to maximum transmission is 0.7585. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       block
_exptl_crystal_F_000             6458
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.886
_refine_diff_density_min         -2.079
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1532
_refine_ls_number_reflns         41481
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0786P)^2^+51.8706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32791
_reflns_number_total             41481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04147h2.cif
_cod_data_source_block           2
_cod_original_cell_volume        11703.0(8)
_cod_database_code               7701995
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.623
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C107-C108
 1.42 with sigma of 0.01
3. Restrained planarity
 C110, C109, C107, C106, N1
 with sigma of 0.1
 N1, C110, C109, C107, C106
 with sigma of 0.1
 N1, C110, C109, C108, C107, C106
 with sigma of 0.1
 C1, C7, N2, C26, C105, C2
 with sigma of 0.1
4. Rigid bond restraints
 Cu10, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cu11) \\sim Ueq, : with sigma of 0.001 and sigma for terminal atoms of
0.002
6. Others
 Fixed Sof: O5AW(0.6) O5BW(0.4)
 Fixed Uiso: C1(0.16927) C2(0.14238) C44(0.1234) C107(0.1276) C108(0.15833)
 C109(0.14952)
7.a Secondary CH2 refined with riding coordinates:
 C105(H10A,H10B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
  C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
 C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
 C43(H43), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
  C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61),
 C62(H62), C63(H63), C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70),
  C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C78(H78),
 C79(H79), C80(H80), C81(H81), C85(H85), C86(H86), C89(H89), C91(H91), C92(H92),
  C93(H93), C94(H94), C95(H95), C99(H99), C100(H100), C107(H107), C108(H108),
 C109(H109), C110(H110)
;
_smtbx_masks_special_details
;   
A solvent mask was calculated and 1045.5 electrons were found in a volume of4690.8\%A^3 in void. This is consistent with the presence of 52[H2O] per formula unit which account for 1040.0 electrons.
;
_shelx_res_checksum              85332
_shelx_fab_checksum              4055
_olex2_submission_special_instructions 'No special instructions were received'