Magnetic double-tartaric bridging mono-lanthanide substituted phosphotungstates with photochromic and switchable luminescence properties
Pengtao Ma; Feng Hu; Rong Wan; Yu Huo; Dongdi Zhang; Jingyang Niu; Jingping Wang; Journal of Materials Chemistry C 4 (2016) 5424–5433; doi:10.1039/C6TC00960C

data_7234833
_publ_section_title
;
 Magnetic double-tartaric bridging mono-lanthanide substituted
 phosphotungstates with photochromic and switchable luminescence
 properties
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              5424
_journal_page_last               5433
_journal_paper_doi               10.1039/C6TC00960C
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         'C8 H4 Er2 O90 P2 W22, 6(C4 H12 N), 10(O)'
_chemical_formula_sum            'C32 H86 Er2 N6 O100 P2 W22'
_chemical_formula_weight         6596.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1047(14)
_cell_length_b                   13.0665(9)
_cell_length_c                   52.158(4)
_cell_measurement_reflns_used    9741
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.39
_cell_volume                     15064.9(18)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0636
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            68411
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.607
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.928
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1492 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.4952.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.908
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11656
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.824
_refine_diff_density_min         -2.011
_refine_diff_density_rms         0.307
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         25957
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0496P)^2^+289.6518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.977
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                17377
_reflns_number_total             25957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Mater-Chem-C-2016-4-5424.cif
_cod_data_source_block           2Er
_cod_database_code               7234833
_shelx_estimated_absorpt_t_max   0.110
_shelx_estimated_absorpt_t_min   0.048
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.67(3) 0.33(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C14 = N2-C15 = N3-C17 = N3-C20
 1.47 with sigma of 0.01
 N1-C9 = N1-C10 = N1-C11 = N1-C12
 1.47 with sigma of 0.01
 N2-C13 = N2-C14 = N2-C15 = N2-C16
 1.47 with sigma of 0.01
 N3-C17 = N3-C18 = N3-C19 = N3-C20
 1.47 with sigma of 0.01
 N4-C21 = N4-C22 = N4-C23 = N4-C24
 1.47 with sigma of 0.01
 N5-C25 = N5-C26 = N5-C27 = N5-C28
 1.47 with sigma of 0.01
 N6-C29 = N6-C30 = N6-C31 = N6-C32
 1.47 with sigma of 0.01
 C4-O69 = C8-O90
 1.3 with sigma of 0.01
 O5W-O69
 2.7 with sigma of 0.02
 C1-C2 \\sim C2-C3 \\sim C3-C4
 with sigma of 0.02
 C5-C6 \\sim C6-C7 \\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
 C13-C14 \\sim C13-C15 \\sim C13-C16 \\sim C14-C15 \\sim C14-C16 \\sim C15-C16
 with sigma of 0.02
 C17-C18 \\sim C17-C19 \\sim C17-C20 \\sim C18-C19 \\sim C18-C20 \\sim C19-C20
 with sigma of 0.02
 C21-C22 \\sim C21-C23 \\sim C21-C24 \\sim C22-C23 \\sim C22-C24 \\sim C23-C24
 with sigma of 0.02
 C25-C26 \\sim C25-C27 \\sim C25-C28 \\sim C26-C27 \\sim C26-C28 \\sim C27-C28
 with sigma of 0.02
 C29-C30 \\sim C29-C31 \\sim C29-C32 \\sim C30-C31 \\sim C30-C32 \\sim C31-C32
 with sigma of 0.02
4. Others
 Fixed Sof: O1W(0.5) O2W(0.5) O8W(0.5) O9W(0.5) O10W(0.5) O11W(0.5) O12W(0.5)
 O13W(0.65) O14W(0.35) O15W(0.5)
 Fixed Uiso: C10(0.22775) C11(0.12905) C20(0.12768) C22(0.12633) C24(0.16361)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7)
5.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;