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_7700924
_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         'O136 P4 Pr3 W34, 3(C4 H12 N), 7(O)'
_chemical_formula_sum            'C12 H36 N3 O143 P4 Pr3 W34'
_chemical_formula_weight         9307.95
_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     dual
_audit_creation_date             2019-08-09
_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                 105.3279(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.252(3)
_cell_length_b                   15.1277(16)
_cell_length_c                   28.898(3)
_cell_measurement_reflns_used    8070
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      2.30
_cell_volume                     10646(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0609
_diffrn_reflns_av_unetI/netI     0.1187
_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       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            53887
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.346
_diffrn_source_type              Microfocus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.060
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1258 before and 0.0606 after correction. The Ratio of minimum to maximum transmission is 0.5343. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8052
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         6.968
_refine_diff_density_min         -2.954
_refine_diff_density_rms         0.468
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1639
_refine_ls_number_reflns         31979
_refine_ls_number_restraints     845
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0601P)^2^+470.1858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1649
_reflns_Friedel_coverage         0.692
_reflns_Friedel_fraction_full    0.691
_reflns_Friedel_fraction_max     0.691
_reflns_number_gt                23751
_reflns_number_total             31979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02710f2.cif
_cod_data_source_block           1917532
_cod_depositor_comments
'Adding full bibliography for 7700923--7700925.cif.'
_cod_original_cell_volume        10646.4(19)
_cod_database_code               7700924
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.162
_shelx_estimated_absorpt_t_min   0.076
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(2)
 0.48(2)
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
 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(P1) \\sim Ueq, Uanis(P2) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(O110) \\sim Ueq,
Uanis(O36) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O79) \\sim Ueq, Uanis(O100)
\\sim Ueq, Uanis(O120) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\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(O16)
\\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O19) \\sim Ueq,
Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq,
Uanis(O27) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O30)
\\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33) \\sim Ueq,
Uanis(O34) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O37)
\\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O40) \\sim Ueq,
Uanis(O41) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O45)
\\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(O47) \\sim Ueq, Uanis(O48) \\sim Ueq,
Uanis(O49) \\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(O52) \\sim Ueq, Uanis(O53)
\\sim Ueq, Uanis(O54) \\sim Ueq, Uanis(O55) \\sim Ueq, Uanis(O56) \\sim Ueq,
Uanis(O57) \\sim Ueq, Uanis(O58) \\sim Ueq, Uanis(O59) \\sim Ueq, Uanis(O60)
\\sim Ueq, Uanis(O61) \\sim Ueq, Uanis(O62) \\sim Ueq, Uanis(O63) \\sim Ueq,
Uanis(O64) \\sim Ueq, Uanis(O65) \\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O67)
\\sim Ueq, Uanis(O68) \\sim Ueq, Uanis(O69) \\sim Ueq, Uanis(O70) \\sim Ueq,
Uanis(O71) \\sim Ueq, Uanis(O72) \\sim Ueq, Uanis(O73) \\sim Ueq, Uanis(O74)
\\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(O76) \\sim Ueq, Uanis(O78) \\sim Ueq,
Uanis(O79) \\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O81) \\sim Ueq, Uanis(O82)
\\sim Ueq, Uanis(O83) \\sim Ueq, Uanis(O84) \\sim Ueq, Uanis(O85) \\sim Ueq,
Uanis(O86) \\sim Ueq, Uanis(O87) \\sim Ueq, Uanis(O88) \\sim Ueq, Uanis(O89)
\\sim Ueq, Uanis(O90) \\sim Ueq, Uanis(O91) \\sim Ueq, Uanis(O93) \\sim Ueq,
Uanis(O94) \\sim Ueq, Uanis(O95) \\sim Ueq, Uanis(O96) \\sim Ueq, Uanis(O97)
\\sim Ueq, Uanis(O98) \\sim Ueq, Uanis(O99) \\sim Ueq, Uanis(O100) \\sim Ueq,
Uanis(O101) \\sim Ueq, Uanis(O102) \\sim Ueq, Uanis(O103) \\sim Ueq,
Uanis(O104) \\sim Ueq, Uanis(O105) \\sim Ueq, Uanis(O106) \\sim Ueq,
Uanis(O107) \\sim Ueq, Uanis(O108) \\sim Ueq, Uanis(O109) \\sim Ueq,
Uanis(O110) \\sim Ueq, Uanis(O111) \\sim Ueq, Uanis(O113) \\sim Ueq,
Uanis(O115) \\sim Ueq, Uanis(O116) \\sim Ueq, Uanis(O117) \\sim Ueq,
Uanis(O118) \\sim Ueq, Uanis(O119) \\sim Ueq, Uanis(O120) \\sim Ueq,
Uanis(O121) \\sim Ueq, Uanis(O122) \\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O2W)
\\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O5W) \\sim Ueq,
Uanis(O6W) \\sim Ueq, Uanis(O7W) \\sim Ueq, Uanis(O8W) \\sim Ueq, Uanis(O9W)
\\sim Ueq, Uanis(O10W) \\sim Ueq, Uanis(O11W) \\sim Ueq, Uanis(O12W) \\sim Ueq,
Uanis(O13W) \\sim Ueq, Uanis(O14W) \\sim Ueq, : with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Others
 Fixed Uiso: N3(0.09655) C1(0.10729) C4(0.12503) C5(0.12932) C7(0.12473)
 C9(0.14246) C10(0.13262) C11(0.14361) C12(0.15423)
6.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              94543
_olex2_submission_special_instructions 'No special instructions were received'