Photocatalysis, terahertz time domain spectroscopy and weak interactions of six polyoxometalate-based lanthanide phosphine oxide complexes
Jin, Guan-Yu; Zhang, Lan; Hu, Fu-Zhen; Hu, Cong; Lu, Yan-Lei; Li, Ying-Yu; Han, Hong-Liang; Liu, Jian-Ming; Yang, Yu-Ping; Jin, Qiong-Hua; Li, Xing-Ru; CrystEngComm  (2022) –; doi:10.1039/D2CE00779G

data_7245142
_publ_section_title
;
 Photocatalysis, terahertz time domain spectroscopy and weak interactions
 of six polyoxometalate-based lanthanide phosphine oxide complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00779G
_journal_year                    2022
_chemical_formula_moiety         'C72 H66 Nd O7 P4, Mo12 O40 P, 4(C2 H3 N)'
_chemical_formula_sum            'C80 H78 Mo12 N4 Nd O47 P5'
_chemical_formula_weight         3297.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-16 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4967(3)
_cell_length_b                   17.7167(3)
_cell_length_c                   27.0552(4)
_cell_measurement_reflns_used    42826
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.84
_cell_measurement_theta_min      5.05
_cell_volume                     10304.0(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1628
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35753
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         3.622
_exptl_absorpt_coefficient_mu    16.833
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_description       block
_exptl_crystal_F_000             6404
_refine_diff_density_max         4.442
_refine_diff_density_min         -5.781
_refine_diff_density_rms         0.370
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         9104
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1610P)^2^+115.3913P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2392
_refine_ls_wR_factor_ref         0.2428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8422
_reflns_number_total             9104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00779g2.cif
_cod_data_source_block           lu-242
_cod_database_code               7245142
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Mo2-O20
 1.646 with sigma of 0.02
 O3-H3A = O3-H3B
 0.85 with sigma of 0.03
 H3A-H3B
 1.35 with sigma of 0.02
 O4-H4A = O4-H4B
 0.85 with sigma of 0.03
 H4A-H4B
 1.35 with sigma of 0.02
3. Rigid bond restraints
 O25, P1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O16) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O21) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O9)
\\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O5) \\sim Ueq,
Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O19) \\sim Ueq,
Uanis(O13) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O25)
\\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O23) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O24) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: H4A(0.5) H4B(0.5) O22(0.5) O23(0.5) O25(0.5) O24(0.5)
6.a Riding coordinates:
 O3(H3A,H3B), O4(H4A,H4B)
6.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C14(H14), C36(H36), C24(H24), C10(H10), C2(H2), C16(H16), C28(H28),
 C6(H6), C33(H33), C34(H34), C4(H4), C17(H17), C35(H35), C26(H26), C20(H20),
 C22(H22), C15(H15), C8(H8), C23(H23), C18(H18), C11(H11), C9(H9), C12(H12),
 C21(H21), C30(H30), C5(H5), C3(H3), C29(H29), C27(H27)
6.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              9777
_shelx_hkl_checksum              47249
_olex2_submission_special_instructions 'No special instructions were received'