Efficient visible-light-driven reduction of hexavalent chromium catalyzed by conjugated organic species modified hourglass-type phosphomolybdate hybrids
Bi, Hao-Xue; Yin, Xiao-Yu; Zhang, Xiu-Juan; Ma, Yuan-Yuan; Han, Zhan-Gang; CrystEngComm 24 (2022) 1002–1009; doi:10.1039/D1CE01467F

data_7244167
_publ_section_title
;
 Efficient visible-light-driven reduction of hexavalent chromium catalyzed
 by conjugated organic species modified hourglass-type phosphomolybdate
 hybrids
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1002
_journal_page_last               1009
_journal_paper_doi               10.1039/D1CE01467F
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety
'Fe2 H4 Mo12 Na2 O67 P8, 2(C12 H13 N2), 2(C20 H18 N2), 4(O)'
_chemical_formula_sum            'C64 H64 Fe2 Mo12 N8 Na2 O71 P8'
_chemical_formula_weight         3637.95
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-09 deposited with the CCDC.	2021-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                105.883(3)
_cell_angle_beta                 99.311(3)
_cell_angle_gamma                92.164(3)
_cell_formula_units_Z            1
_cell_length_a                   11.853(2)
_cell_length_b                   14.016(2)
_cell_length_c                   16.932(3)
_cell_measurement_reflns_used    4710
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.34
_cell_volume                     2659.9(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16442
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.258
_diffrn_reflns_theta_min         1.680
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.870
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5391
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0725 before and 0.0434 after correction.
The Ratio of minimum to maximum transmission is 0.7229.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       plate
_exptl_crystal_F_000             1770
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.935
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         12017
_refine_ls_number_restraints     1020
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1104P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9080
_reflns_number_total             12017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01467f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7244167--7244170.cif.'
_cod_database_code               7244167
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C46 \\sim C47 \\sim C48 \\sim
C50 \\sim C52 \\sim C55 \\sim C60 \\sim C4 \\sim C0AA \\sim C6 \\sim C7 \\sim
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C14 \\sim C15 \\sim C16 \\sim
C17 \\sim C18 \\sim C19 \\sim C21 \\sim C22 \\sim C25 \\sim C26 \\sim C5 \\sim
N2 \\sim N1 \\sim N3 \\sim N4: within 3.8A with sigma of 0.04 and sigma for
terminal atoms of 0.02
Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3WA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O3W(0.5) O4W(0.5) H4WA(0.5) H4WB(0.5) O3WA(0.5)
4.a Rotating group:
 N1(H1A,H1B), O4W(H4WA,H4WB)
4.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C42(H42), C46(H46), C48(H48), C50(H50), C52(H52), C55(H55),
 C60(H60), N3(H3), C7(H7), C9(H9), C11(H11), C12(H12), N4(H4), C14(H14),
 C15(H15), C18(H18), C22(H22), C25(H25), C26(H26)
4.c Tetrahedral OH refined with riding coordinates:
 O2(H2)
4.d Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              75519
_shelx_hkl_checksum              5493
_olex2_submission_special_instructions 'No special instructions were received'