A luminescent polyoxoniobate lanthanide derivative {Eu3(H2O)9[Nb48O138(H2O)6]}(27-) .
Chen, Shumin; Ma, Pengtao; Luo, Huihui; Wang, Yangyang; Niu, Jingyang; Wang, Jingping; Chemical communications (Cambridge, England) 53 (2017) 3709–3712; doi:10.1039/c7cc00591a

data_7119758
_publ_section_title
;
 A luminescent polyoxoniobate lanthanide derivative
 {Eu3(H2O)9[Nb48O138(H2O)6]}(27-)&#x2009;.
;
_journal_issue                   26
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3709
_journal_page_last               3712
_journal_paper_doi               10.1039/c7cc00591a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'Eu3 K3 Nb48 O153, 6(C H6 N3), 21(O)'
_chemical_formula_sum            'C6 H108 Eu3 K3 N18 Nb48 O174'
_chemical_formula_weight         8249.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-01-13 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6425(12)
_cell_length_b                   38.357(2)
_cell_length_c                   45.950(3)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.33
_cell_volume                     32846(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            84601
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.702
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.272
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0982 before and 0.0498 after correction.
The Ratio of minimum to maximum transmission is 0.6717.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             15504
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.422
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         29156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+1260.6422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.2048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22402
_reflns_number_total             29156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00591a2.cif
_cod_data_source_block           njy1
_cod_depositor_comments          'Adding full bibliography for 7119758.cif.'
_cod_original_cell_volume        32846(4)
_cod_database_code               7119758
_shelx_estimated_absorpt_t_max   0.590
_shelx_estimated_absorpt_t_min   0.409
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: Eu2(0.5) K2(0.5) O7W(0.5) O8W(0.5) O9W(0.5) O15W(0.5) O16W(0.5)
 O17W(0.5) O18W(0.5) O19W(0.5) O20W(0.5) O21W(0.5) O22W(0.5) O23W(0.5)
 O24W(0.5) O25W(0.5) O26W(0.5)
3.a X=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)
;
_shelx_res_checksum              4934
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'