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_7244170
_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
'Mo12 Na2 O70 P8 Zn2, 2(C12 H13 N2), 2(C20 H14 N2)'
_chemical_formula_sum            'C64 H60 K2 Mo12 N8 Na2 O69 P8 Zn'
_chemical_formula_weight         3633.79
_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             2020-11-11
_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                75.738(3)
_cell_angle_beta                 80.286(3)
_cell_angle_gamma                89.388(3)
_cell_formula_units_Z            1
_cell_length_a                   12.079(2)
_cell_length_b                   13.620(2)
_cell_length_c                   17.023(3)
_cell_measurement_reflns_used    7466
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.22
_cell_volume                     2673.9(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_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\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  0.0269
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15654
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.207
_diffrn_reflns_theta_min         1.543
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5479
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0984 before and 0.0411 after correction.
The Ratio of minimum to maximum transmission is 0.7347.
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    2.257
_exptl_crystal_description       block
_exptl_crystal_F_000             1766
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.274
_refine_diff_density_min         -2.438
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         11790
_refine_ls_number_restraints     840
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0688P)^2^+31.6457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8479
_reflns_number_total             11790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01467f2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7244167--7244170.cif.'
_cod_original_cell_volume        2674.0(8)
_cod_database_code               7244170
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.703
_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
2. Uiso/Uaniso restraints and constraints
C4 \\sim C6 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C14 \\sim C15 \\sim
C17 \\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 C40 \\sim N1 \\sim N2 \\sim
N3 \\sim N4: within 3.8A with sigma of 0.04 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Zn2(0.25) Zn2A(0.25)
4.a Rotating group:
 N3(H3A,H3B)
4.b :
 C1(C40,C36,C35,N4,C34)
4.c Aromatic/amide H refined with riding coordinates:
 C6(H6), N2(H2), C10(H10), C11(H11), C15(H15), C17(H17), C20(H20), C21(H21),
 C22(H22), C23(H23), C25(H25), C27(H27), C28(H28), C31(H31), C33(H33), C37(H37),
  C38(H38), C1(H1), C40(H40)
4.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              71139
_shelx_hkl_checksum              36828
_shelx_fab_checksum              6078
_olex2_submission_special_instructions 'No special instructions were received'