A series of rare-earth phosphine-oxygen complexes containing [PW12O40]3− with highly efficient photocatalytic degradation of MB
Li, Ying-Yu; Qiu, Qi-Ming; Fan, Si-Jie; Xu, Jian-Jie; Mou, Wen-Long; Hou, Chuan-Bing; Liu, Min; Yang, Yu-Ping; Dai, Li-Xiong; Han, Hong-Liang; Jin, Qiong-Hua; CrystEngComm 26 (2024) 5809–5819; doi:10.1039/D4CE00851K

data_7249343
_publ_section_title
;
 A series of rare-earth phosphine-oxygen complexes containing
 [PW12O40]3&#x2212; with highly efficient photocatalytic degradation of MB
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              5809
_journal_page_last               5819
_journal_paper_doi               10.1039/D4CE00851K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '0.043(O40 P W12), 0.043(C42 Ho O20 P6)'
_chemical_formula_sum            'C Cl Ho O P W'
_chemical_formula_weight         443.21
_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_primary     dual
_audit_creation_date             2023-02-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-03-10 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                104.628(2)
_cell_angle_beta                 94.579(2)
_cell_angle_gamma                116.295(3)
_cell_formula_units_Z            46
_cell_length_a                   15.5991(5)
_cell_length_b                   16.9243(5)
_cell_length_c                   21.7605(5)
_cell_measurement_reflns_used    21901
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.9590
_cell_measurement_theta_min      2.3790
_cell_volume                     4860.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -56.00  17.00   0.50    1.98    --    3.36 -57.00   0.00  146
  2  \w    -63.00  11.00   0.50    1.98    --    3.36 -38.00  90.00  148
  3  \w    -37.00  28.00   0.50    1.98    --    3.36 -81.00  58.00  130
  4  \w    -21.00  42.00   0.50    1.98    --    3.36  81.00-178.00  126
  5  \w    -31.00  27.00   0.50    1.98    --   -6.72  81.00-178.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0040180000
_diffrn_orient_matrix_UB_12      0.0402301000
_diffrn_orient_matrix_UB_13      0.0150328000
_diffrn_orient_matrix_UB_21      -0.0402240000
_diffrn_orient_matrix_UB_22      -0.0146789000
_diffrn_orient_matrix_UB_23      -0.0256605000
_diffrn_orient_matrix_UB_31      -0.0327159000
_diffrn_orient_matrix_UB_32      -0.0245855000
_diffrn_orient_matrix_UB_33      0.0175693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.1238
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51815
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    46.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    6.966
_exptl_crystal_F_000             8602
_refine_diff_density_max         8.026
_refine_diff_density_min         -4.968
_refine_diff_density_rms         0.671
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         19876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1644
_refine_ls_R_factor_gt           0.1400
_refine_ls_shift/su_max          1.013
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+2672.4285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3610
_refine_ls_wR_factor_ref         0.3686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14998
_reflns_number_total             19876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00851k21.cif
_cod_data_source_block           exp_1650_auto
_cod_depositor_comments
'Adding full bibliography for 7249339--7249349.cif.'
_cod_database_code               7249343
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Ho Cl C P O W'
_olex2_refinement_description
;
1. Others
 Fixed Sof: O24(0.5) O25(0.5) O43(0.5) O46(0.5) O29(0.5) O30(0.5) O26(0.5)
 O28(0.5)
;
_shelx_res_checksum              74811
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.579
_oxdiff_exptl_absorpt_empirical_full_min 0.216