An Unprecedented 3D Architecture Based on Nb/W Mixed-Addendum Polyoxometalate and Lanthanide-Organic Complex: Synthesis, Crystal Structure and Properties
Yang, Mei-Si; Chen, Wei-Chao; Qin, Chao; Yao, Wei; Yin, Ying-Xue; Su, Zhong-Min; New J. Chem. 41 (2017) 10532–10536; doi:10.1039/C7NJ02011B

data_7056502
_publ_section_title
;
 An Unprecedented 3D Architecture Based on Nb/W Mixed-Addendum
 Polyoxometalate and Lanthanide-Organic Complex: Synthesis, Crystal
 Structure and Properties
;
_journal_issue                   19
_journal_name_full               'New J. Chem.'
_journal_page_first              10532
_journal_page_last               10536
_journal_paper_doi               10.1039/C7NJ02011B
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C36 H24 La8 N6 Nb9 O164 Si3 W27, 14(O)'
_chemical_formula_sum            'C36 H27 La8 N6 Nb9 O172 Si3 W27'
_chemical_formula_weight         10291.32
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-17 deposited with the CCDC.
2017-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   23.4764(7)
_cell_length_b                   23.4764(7)
_cell_length_c                   12.1560(6)
_cell_measurement_reflns_used    43287
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     5802.1(4)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43287
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         1.952
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    15.288
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4526
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.722
_refine_diff_density_min         -2.002
_refine_diff_density_rms         0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9601
_refine_ls_number_restraints     825
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0478P)^2^+188.1340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7980
_reflns_number_total             9601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02011b2.cif
_cod_data_source_block           p-3_sq
_cod_database_code               7056502
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O23-C6 = O24-C6 = O26-C6' = O25-C6'
 1.25 with sigma of 0.02
 C4'-C6' = C4-C6
 1.45 with sigma of 0.02
 O2W-La2
 2.6 with sigma of 0.01
 O24-O23 \\sim O25-O26
 with sigma of 0.001
 C4-C6 \\sim C4'-C6'
 with sigma of 0.001
 O23-C6 \\sim O24-C6 \\sim O25-C6' \\sim O26-C6'
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C1 \\sim C2 \\sim C3 \\sim C6 \\sim C4' \\sim C3' \\sim C2'
\\sim C1' \\sim C5' \\sim C6' \\sim N1 \\sim N1': within 3.8A with sigma of
0.03 and sigma for terminal atoms of 0.03
Uanis(C6') \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(C4')
\\sim Ueq, Uanis(C3') \\sim Ueq, Uanis(C5') \\sim Ueq, Uanis(C2') \\sim Ueq,
Uanis(N1') \\sim Ueq, Uanis(C1') \\sim Ueq, : with sigma of 0.01 and sigma for
terminal atoms of 0.005
Uanis(O7W) \\sim Ueq, Uanis(O5W) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O6W)
\\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(O8) \\sim Ueq,
Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O13) \\sim Ueq,
Uanis(O4) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O16) \\sim Ueq:
with sigma of 0.03 and sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O5W)
\\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.001
Uanis(W4) = Uanis(Nb4)
Uanis(W5) = Uanis(Nb5)
Uanis(W6) = Uanis(Nb6)
4. Rigid body (RIGU) restrains
 O25, O26, C4', C3', H3', C2', H2', C1', H1', N1', C5', H5', C6'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O23, O24, C4, C5, H5, N1, C1, H1, C2, H2, C3, H3, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O17(0.5) O18(0.5) O19(0.5) O22(0.5) W4(0.5) W5(0.5) W6(0.5)
 La1(0.9) O23(0.7) O24(0.7) C4(0.7) C5(0.7) H5(0.7) N1(0.7) C1(0.7) H1(0.7)
 C2(0.7) H2(0.7) C3(0.7) H3(0.7) C6(0.7) La1'(0.1) Nb4(0.5) Nb5(0.5) Nb6(0.5)
 O25(0.3) O26(0.3) C4'(0.3) C3'(0.3) H3'(0.3) C2'(0.3) H2'(0.3) C1'(0.3)
 H1'(0.3) N1'(0.3) C5'(0.3) H5'(0.3) C6'(0.3)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C1(H1), C2(H2), C3(H3), C3'(H3'), C2'(H2'), C1'(H1'), C5'(H5')
6.b Fitted hexagon refined as free rotating group:
 C4(C5,N1,C1,C2,C3), C4'(C3',C2',C1',N1',C5')
;
_shelx_res_checksum              65552
_shelx_fab_checksum              98793
_olex2_submission_special_instructions 'No special instructions were received'