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_7244169
_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
'Co2 Mo12 Na2 O66 P8, 2(C12 H13 N2), 2(C20 H18 N2), 4(O)'
_chemical_formula_sum            'C64 H62 Co2 Mo12 N8 Na2 O70 P8'
_chemical_formula_weight         3626.09
_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
_audit_creation_date             2020-10-15
_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                105.9222(13)
_cell_angle_beta                 99.3799(14)
_cell_angle_gamma                92.0586(15)
_cell_formula_units_Z            1
_cell_length_a                   11.8560(10)
_cell_length_b                   14.0079(12)
_cell_length_c                   16.8886(14)
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.34
_cell_volume                     2651.5(4)
_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)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13390
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.275
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0476 before and 0.0324 after correction.
The Ratio of minimum to maximum transmission is 0.9108.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1762
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.246
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         9277
_refine_ls_number_restraints     750
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0713P)^2^+15.6470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7221
_reflns_number_total             9277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01467f2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7244167--7244170.cif.'
_cod_database_code               7244169
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.701
_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
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C57 \\sim
C58 \\sim C61 \\sim C62 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C69 \\sim
C70 \\sim C75 \\sim C8 \\sim C3 \\sim C4 \\sim C2 \\sim C1 \\sim C5: within
3.8A with sigma of 0.04 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C5) \\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(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Rotating group:
 N2(H2A,H2B)
3.b :
 N4(C4,C8,C1,C2,C3)
3.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C42(H42), C45(H45), C46(H46), C48(H48), C50(H50), C51(H51),
 C54(H54), C55(H55), N3(H3), C57(H57), C61(H61), C62(H62), C64(H64), C66(H66),
 C67(H67), C70(H70), N4(H4), C1(H1), C2(H2)
3.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C75(H75A,H75B,H75C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              26828
_shelx_hkl_checksum              88561
_olex2_submission_special_instructions 'No special instructions were received'