Synthesis, characterization, and photoluminescence properties of three two-dimensional lanthanide-containing Dawson-type polyoxometalates.
Wu, Hechen; Zhi, Minna; Chen, Chunli; Zhu, Yanhong; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13850–13857; doi:10.1039/c9dt02710f

data_7700923
_publ_section_title
;
 Synthesis, characterization, and photoluminescence properties of three
 two-dimensional lanthanide-containing Dawson-type polyoxometalates.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13850
_journal_page_last               13857
_journal_paper_doi               10.1039/c9dt02710f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'La3 O136 P4 W34, 3(C4 H12 N), 5(O)'
_chemical_formula_sum            'C12 H36 La3 N3 O141 P4 W34'
_chemical_formula_weight         9269.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-14 deposited with the CCDC.    2019-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.488(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.109(2)
_cell_length_b                   14.9811(13)
_cell_length_c                   28.785(2)
_cell_measurement_reflns_used    8762
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.69
_cell_measurement_theta_min      2.32
_cell_volume                     10434.6(14)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.1034
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            52905
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.718
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.359
_exptl_absorpt_coefficient_mu    19.360
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1397 before and 0.0561 after correction. The Ratio of minimum to maximum transmission is 0.5687. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.950
_exptl_crystal_description       block
_exptl_crystal_F_000             8008
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.043
_refine_diff_density_min         -2.341
_refine_diff_density_rms         0.397
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.435(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1630
_refine_ls_number_reflns         26683
_refine_ls_number_restraints     2558
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+116.4672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.438
_reflns_Friedel_fraction_full    0.438
_reflns_Friedel_fraction_max     0.438
_reflns_number_gt                21171
_reflns_number_total             26683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02710f2.cif
_cod_data_source_block           1917530
_cod_depositor_comments
'Adding full bibliography for 7700923--7700925.cif.'
_cod_original_cell_volume        10434.5(15)
_cod_database_code               7700923
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.187
_shelx_estimated_absorpt_t_min   0.081
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.565(19)
 0.435(19)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-C1 = N1-C2 = N1-C3 = N1-C4
 1.5 with sigma of 0.01
 N2-C5 = N2-C6 = N2-C7 = N2-C8
 1.5 with sigma of 0.01
 N3-C9 = N3-C10 = N3-C11 = N3-C12
 1.5 with sigma of 0.02
 O2W-O18W
 2.6 with sigma of 0.02
 C1-C2 \\sim C1-C3 \\sim C1-C4 \\sim C2-C3 \\sim C2-C4 \\sim C3-C4
 with sigma of 0.02
 C5-C6 \\sim C5-C7 \\sim C5-C8 \\sim C6-C7 \\sim C6-C8 \\sim C7-C8
 with sigma of 0.02
 C9-C10 \\sim C9-C11 \\sim C9-C12 \\sim C10-C11 \\sim C10-C12 \\sim C11-C12
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(P1) \\sim Ueq, Uanis(P2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Uiso: N3(0.09655) C1(0.10729) C3(0.13812) C4(0.12503) C5(0.12932)
 C7(0.12473) C9(0.14246) C10(0.13262) C11(0.14361) C12(0.14423)
7.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              70836
_olex2_submission_special_instructions 'No special instructions were received'