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_7244168
_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
'Mn2 Mo12 Na2 O66 P8, 2(C12 H13 N2), 2(C20 H13 N2 O), 3(O)'
_chemical_formula_sum            'C64 H52 Mn2 Mo12 N8 Na4 O70 P8'
_chemical_formula_weight         3654.01
_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             2021-04-09
_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                106.8435(17)
_cell_angle_beta                 100.0004(16)
_cell_angle_gamma                91.8117(16)
_cell_formula_units_Z            1
_cell_length_a                   11.8092(12)
_cell_length_b                   14.1430(15)
_cell_length_c                   17.0587(19)
_cell_measurement_reflns_used    5293
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.33
_cell_volume                     2675.3(5)
_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 0.987
_diffrn_measured_fraction_theta_max 0.916
_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  0.0230
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16597
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.510
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.831
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6123
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0516 before and 0.0320 after correction.
The Ratio of minimum to maximum transmission is 0.8211.
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    2.268
_exptl_crystal_description       block
_exptl_crystal_F_000             1770
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.561
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         12158
_refine_ls_number_restraints     726
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0758P)^2^+10.8864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9439
_reflns_number_total             12158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01467f2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7244167--7244170.cif.'
_cod_database_code               7244168
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.711
_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
C38 \\sim C39 \\sim C41 \\sim C42 \\sim C43 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C51 \\sim C55 \\sim C56 \\sim C2AA \\sim C3AA \\sim C6 \\sim C7 \\sim
C8 \\sim C0AA \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim
C19 \\sim C1AA \\sim C1 \\sim C4AA \\sim C5AA \\sim C4 \\sim C3 \\sim C2:
within 3.8A with sigma of 0.04 and sigma for terminal atoms of 0.02
Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9W) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
3. Others
 Fixed Sof: O3W(0.5)
4.a Rotating group:
 N2(H2A,H2B)
4.b :
 C3(C4,C17,C4AA,N4,C5AA)
4.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C41(H41), C42(H42), C47(H47), C48(H48), C49(H49), C55(H55),
 C56(H56), N3(H3), C2AA(H2AA), C8(H8), C13(H13), C15(H15), C16(H16), C19(H19),
 C1AA(H1AA), C3(H3A), C4(H4)
4.d Idealised Me refined as rotating group:
 N1(H1D,H1E,H1F), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              6002
_shelx_hkl_checksum              97849
_olex2_submission_special_instructions 'No special instructions were received'