Efficient dye degradation and THz spectra of {PMo12} based rare earth phosphine oxide complexes
Hu, Cong; Li, Ying-Yu; Qiu, Qi-Ming; Han, Hong-Liang; Gu, Chao-Yue; Yang, Yu-Ping; Dai, Li-Xiong; Jin, Qiong-Hua; CrystEngComm  (2022) –; doi:10.1039/D2CE00989G

data_7245613
_publ_section_title
;
 Efficient dye degradation and THz spectra of {PMo12} based rare earth
 phosphine oxide complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00989G
_journal_year                    2022
_chemical_formula_moiety
'C40 H85 Eu O24 P8, 2(Mo6 O20 P0.5), 2(C2 H3 N)'
_chemical_formula_sum            'C44 H91 Eu Mo12 N2 O64 P9'
_chemical_formula_weight         3254.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-15 deposited with the CCDC.	2022-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                100.341(3)
_cell_angle_beta                 95.132(2)
_cell_angle_gamma                114.438(4)
_cell_formula_units_Z            2
_cell_length_a                   13.7674(14)
_cell_length_b                   14.6533(15)
_cell_length_c                   27.613(3)
_cell_measurement_reflns_used    4699
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.944
_cell_measurement_theta_min      2.438
_cell_volume                     4905.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.1269
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24424
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         1.904
_exptl_absorpt_coefficient_mu    2.356
_exptl_absorpt_correction_T_max  0.5384
_exptl_absorpt_correction_T_min  0.4760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3166
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.310
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1223
_refine_ls_number_reflns         17038
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0844P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8244
_reflns_number_total             17038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00989g2.cif
_cod_data_source_block           210111g
_cod_original_cell_volume        4905.0(9)
_cod_database_code               7245613
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.538
_shelx_estimated_absorpt_t_min   0.476
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C41 = N2-C43
 1.15 with sigma of 0.01
 C41-C42 = C43-C44
 1.48 with sigma of 0.01
 C31-C32 = C33-C34 = C35-C36 = C37-C38 = C39-C40
 1.53 with sigma of 0.01
 O20-C33 = O21-C35 = O23-C37 = O24-C39
 1.43 with sigma of 0.01
 C21-C22 = C23-C24 = C25-C26 = C27-C28 = C29-C30
 1.53 with sigma of 0.01
 O14-C23 = O15-C25 = O17-C27 = O18-C29
 1.43 with sigma of 0.01
 C11-C12 = C13-C14 = C15-C16 = C17-C18 = C19-C20
 1.53 with sigma of 0.01
 O8-C13 = O9-C15 = O11-C17 = O12-C19
 1.43 with sigma of 0.01
 C1-C2 = C3-C4 = C5-C6 = C7-C8 = C9-C10
 1.53 with sigma of 0.01
 O2-C3 = O3-C5 = O5-C7 = O6-C9
 1.43 with sigma of 0.01
 P10-O47 = P10-O48 = P10-O49 = P10-O50
 1.58 with sigma of 0.01
 P1-O3 = P9-O25 = P9-O26 = P9-O27 = P9-O28
 1.58 with sigma of 0.01
 O3-C6
 2.46 with sigma of 0.02
 O21-C35
 2.46 with sigma of 0.0005
 C4-C3
 1.535 with sigma of 0.0005
3. Rigid bond restraints
 C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C19, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim N1 \\sim N2: within 3.8A with sigma of 0.02
and sigma for terminal atoms of 0.04
5. Others
 Fixed Sof: O25(0.5) O26(0.5) O27(0.5) O28(0.5) O47(0.5) O48(0.5) O49(0.5)
 O50(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C13(H13A,H13B), C15(H15A,
 H15B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B),
 C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B),
  C37(H37A,H37B), C39(H39A,H39B)
6.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C),
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C11(H11), C12(H12), C22(H22), C32(H32)
;
_shelx_res_checksum              46781
_shelx_hkl_checksum              11269
_olex2_submission_special_instructions 'No special instructions were received'