Synthesis, structural characterization, DFT and molecular dynamics simulations of dinuclear (μ-hydroxo)-bridged triethanolamine copper(II) complexes: efficient candidates towards visible light-mediated photo-Fenton degradation of organic dyes.
Chauhan, Chetan; Tanuj, ?; Kumar, Rajesh; Kumar, Jitendra; Sharma, Subhash; Benmansour, Samia; Kumar, Santosh; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13638–13661; doi:10.1039/d4dt01463d

data_7716793
_publ_section_title
;
 Synthesis, structural characterization, DFT and molecular dynamics
 simulations of dinuclear (&#x3bc;-hydroxo)-bridged triethanolamine
 copper(II) complexes: efficient candidates towards visible light-mediated
 photo-Fenton degradation of organic dyes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13638
_journal_page_last               13661
_journal_paper_doi               10.1039/d4dt01463d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H34 Cu2 F4 N2 O10, 2(H2 O)'
_chemical_formula_sum            'C26 H38 Cu2 F4 N2 O12'
_chemical_formula_weight         773.66
_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     dual
_audit_creation_date             2023-02-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                74.282(2)
_cell_angle_beta                 89.651(2)
_cell_angle_gamma                65.016(3)
_cell_formula_units_Z            1
_cell_length_a                   7.5237(2)
_cell_length_b                   8.2475(2)
_cell_length_c                   14.3873(4)
_cell_measurement_reflns_used    4538
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      66.5150
_cell_measurement_theta_min      6.0560
_cell_volume                     772.93(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -38.00   5.00   0.50    0.10    --  -46.98  38.00-120.00   86
  2  \w    -12.00  29.00   0.50    0.10    --  -46.98  19.00 -90.00   82
  3  \w     -2.00  29.00   0.50    0.10    --  -46.98  19.00 -60.00   62
  4  \w     -7.00  29.00   0.50    0.10    --  -46.98  19.00 150.00   72
  5  \w   -108.00 -82.00   0.50    0.10    --  -46.98   0.00  90.00   52
  6  \w    -35.00  26.00   0.50    0.10    --  -46.98  38.00  30.00  122
  7  \w    -70.00 -30.00   0.50    0.25    -- -103.00  61.00-120.00   80
  8  \w    -69.00 -32.00   0.50    0.25    -- -103.00  61.00-180.00   74
  9  \w    -67.00 -30.00   0.50    0.25    -- -103.00  61.00 -90.00   74
 10  \w    -64.00 -39.00   0.50    0.25    -- -103.00  61.00   0.00   50
 11  \w    -71.00 -33.00   0.50    0.25    -- -103.00 125.00  60.00   76
 12  \w   -104.00 -78.00   0.50    0.25    -- -103.00 125.00  60.00   52
 13  \w    -66.00 -21.00   0.50    0.10    --  -46.98  84.00 -93.00   90
 14  \w    -15.00  26.00   0.50    0.10    --  -46.98  84.00 -93.00   82
 15  \w    -97.00 -67.00   0.50    0.25    -- -103.00  84.00 -93.00   60
 16  \w   -114.00 -89.00   0.50    0.25    -- -103.00 -15.00  30.00   50
 17  \w   -156.00-102.00   0.50    0.25    -- -103.00 -84.00 146.00  108
 18  \w   -148.00-123.00   0.50    0.25    -- -103.00 -15.00  30.00   50
 19  \w   -170.00 -75.00   0.50    0.25    -- -103.00-125.00 -60.00  190
 20  \w   -174.00 -91.00   0.50    0.25    -- -103.00 -30.00-180.00  166
 21  \w    -23.00  16.00   0.50    0.10    --   46.98 -19.00-120.00   78
 22  \w     39.00  76.00   0.50    0.25    --  106.08 -61.00-150.00   74
 23  \w     34.00  65.00   0.50    0.25    --  106.08 -61.00 -60.00   62
 24  \w     37.00  68.00   0.50    0.25    --  106.08 -61.00 -30.00   62
 25  \w     37.00  62.00   0.50    0.25    --  106.08 -61.00   0.00   50
 26  \w     76.00 108.00   0.50    0.25    --  106.08-125.00   0.00   64
 27  \w     37.00 100.00   0.50    0.25    --  106.08 -95.00 -30.00  126
 28  \w     40.00  71.00   0.50    0.25    --  106.08-125.00   0.00   62
 29  \w     16.00  52.00   0.50    0.10    --   46.98 -84.00 146.00   72
 30  \w    -20.00  12.00   0.50    0.10    --   46.98 -84.00 146.00   64
 31  \w     36.00 103.00   0.50    0.25    --  106.08 -95.00  60.00  134
 32  \w     62.00 109.00   0.50    0.25    --  106.08 -84.00 146.00   94
 33  \w     55.00 104.00   0.50    0.25    --  106.08 -95.00 150.00   98
 34  \w     87.00 157.00   0.50    0.25    --  106.08  84.00 -93.00  140
 35  \w    108.00 176.00   0.50    0.25    --  106.08  30.00 -30.00  136
 36  \w    140.00 166.00   0.50    0.25    --  106.08   0.00-150.00   52
;
_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      0.0304239000
_diffrn_orient_matrix_UB_12      -0.0764433000
_diffrn_orient_matrix_UB_13      -0.0883251000
_diffrn_orient_matrix_UB_21      -0.2154891000
_diffrn_orient_matrix_UB_22      0.1352670000
_diffrn_orient_matrix_UB_23      -0.0437441000
_diffrn_orient_matrix_UB_31      0.0668527000
_diffrn_orient_matrix_UB_32      0.1496824000
_diffrn_orient_matrix_UB_33      -0.0534102000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7737
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.664
_diffrn_reflns_theta_max         66.664
_diffrn_reflns_theta_min         6.080
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       block
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0301P)^2^+0.4211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2459
_reflns_number_total             2716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01463d2.cif
_cod_data_source_block           crys502a
_cod_depositor_comments
'Adding full bibliography for 7716793--7716795.cif.'
_cod_database_code               7716793
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.788
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C13(H13A,H13B), C11(H11A,H11B), C12(H12A,H12B), C16(H16A,
 H16B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5)
2.d Idealised tetrahedral OH refined as rotating group:
 O12(H12), O13(H13)
;
_shelx_res_checksum              11499
_olex2_submission_original_sample_id A-TEA
_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 1.916
_oxdiff_exptl_absorpt_empirical_full_min 0.596