A large copper-niobate cluster with the pagoda-shaped subunit {Nb<sub>20</sub>O<sub>59</sub>}.
Liang, Zhijie; Qiao, Yuanyuan; Li, Xue; Ma, Pengtao; Niu, Jingyang; Wang, Jingping; Chemical communications (Cambridge, England) 57 (2021) 3999–4002; doi:10.1039/d1cc00758k

data_7128042
_publ_section_title
;
 A large copper-niobate cluster with the pagoda-shaped subunit
 {Nb<sub>20</sub>O<sub>59</sub>}.
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3999
_journal_page_last               4002
_journal_paper_doi               10.1039/d1cc00758k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C16 H64 Cu8 K20 N16 Na19 Nb144 O442, 36(O)'
_chemical_formula_sum            'C16 H64 Cu8 K20 N16 Na19 Nb144 O478'
_chemical_formula_weight         23235.00
_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     dual
_audit_creation_date             2021-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-15 deposited with the CCDC.	2021-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   39.8703(2)
_cell_length_b                   28.15080(10)
_cell_length_c                   63.1542(3)
_cell_measurement_reflns_used    103828
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.4750
_cell_measurement_theta_min      2.7840
_cell_volume                     70803.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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      200.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            286571
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.672
_diffrn_reflns_theta_min         2.219
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.180
_exptl_crystal_description       block
_exptl_crystal_F_000             43284
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.949
_refine_diff_density_min         -2.242
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6227
_refine_ls_number_reflns         135419
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0835P)^2^+2179.8616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                102810
_reflns_number_total             135419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00758k2.cif
_cod_data_source_block           njy1
_cod_depositor_comments          'Adding full bibliography for 7128042.cif.'
_cod_database_code               7128042
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.292
_shelx_estimated_absorpt_t_min   0.139
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 O70W-O34W
 2.65 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq, Uanis(O17W) \\sim Ueq, Uanis(O20W) \\sim Ueq, Uanis(O35W)
\\sim Ueq, Uanis(O38W) \\sim Ueq, Uanis(O43W) \\sim Ueq, Uanis(O44W) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na3) \\sim Ueq, Uanis(O12W) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(Na19) \\sim Ueq, Uanis(Na14) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.016
4. Others
 Fixed Sof: Na19(0.5) Na20(0.5) O48W(0.5) O62W(0.5) O63W(0.5) O64W(0.5)
 O65W(0.5) O66W(0.5) O67W(0.5) O68W(0.5) O69W(0.5) O71W(0.5) O72W(0.5)
 O73W(0.5) O74W(0.5) O75W(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 N7(H7A,H7B), N8(H8A,H8B), N9(H9A,H9B), N10(H10A,H10B), N11(H11A,H11B),
 N12(H12A,H12B), N13(H13A,H13B), N14(H14A,H14B), N15(H15A,H15B), N16(H16A,H16B),
  C1(H1C,H1D), C2(H2C,H2D), C3(H3C,H3D), C4(H4C,H4D), C5(H5C,H5D), C6(H6C,H6D),
 C7(H7C,H7D), C8(H8C,H8D), C9(H9C,H9D), C10(H10C,H10D), C11(H11C,H11D),
 C12(H12C,H12D), C13(H13C,H13D), C14(H14C,H14D), C15(H15C,H15D), C16(H16C,H16D)
;
_shelx_res_checksum              84952
_shelx_fab_checksum              62245
_olex2_submission_special_instructions 'No special instructions were received'