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_7716794
_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 H36 Cl2 Cu2 N2 O10, 2(H2 O)'
_chemical_formula_sum            'C26 H40 Cl2 Cu2 N2 O12'
_chemical_formula_weight         770.58
_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             2024-06-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                74.462(4)
_cell_angle_beta                 88.045(4)
_cell_angle_gamma                71.119(4)
_cell_formula_units_Z            1
_cell_length_a                   7.4656(4)
_cell_length_b                   7.9965(4)
_cell_length_c                   14.2307(5)
_cell_measurement_reflns_used    4497
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      66.4470
_cell_measurement_theta_min      5.9850
_cell_volume                     773.17(7)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -65.00 -32.00   0.50    0.10    -- -103.00  61.00 150.00   66
  2  \w    -63.00 -30.00   0.50    0.10    -- -103.00  61.00 120.00   66
  3  \w    -63.00 -30.00   0.50    0.10    -- -103.00  61.00 -60.00   66
  4  \w    -25.00  25.00   0.50    0.05    --  -46.98  47.00 -51.00  100
  5  \w    -13.00  12.00   0.50    0.05    --  -46.98  19.00-180.00   50
  6  \w    -25.00  22.00   0.50    0.05    --   46.98 -19.00   0.00   94
  7  \w    -25.00  39.00   0.50    0.05    --   46.98 -77.00 -30.00  128
  8  \w     -1.00  42.00   0.50    0.05    --   46.98 -47.00 159.00   86
  9  \w    100.00 137.00   0.50    0.10    --  106.08 125.00 120.00   74
 10  \w    148.00 174.00   0.50    0.10    --  106.08 125.00 120.00   52
 11  \w     42.00  75.00   0.50    0.10    --  106.08 -61.00 -60.00   66
 12  \w     73.00 125.00   0.50    0.10    --  106.08 -77.00  30.00  104
 13  \w     34.00  60.00   0.50    0.10    --  106.08 -77.00  30.00   52
 14  \w    101.00 127.00   0.50    0.10    --  106.08  47.00 -51.00   52
 15  \w    128.00 156.00   0.50    0.10    --  106.08  47.00 -51.00   56
 16  \w    102.00 152.00   0.50    0.10    --  106.08  45.00-120.00  100
 17  \w    127.00 177.00   0.50    0.10    --  106.08  61.00-150.00  100
 18  \w     91.00 123.00   0.50    0.10    --  106.08  61.00-150.00   64
 19  \w     36.00  94.00   0.50    0.05    --   46.98  47.00 -51.00  116
 20  \w    111.00 136.00   0.50    0.10    --  106.08  15.00  90.00   50
 21  \w    140.00 178.00   0.50    0.10    --  106.08  15.00  90.00   76
 22  \w    108.00 167.00   0.50    0.10    --  106.08   0.00  30.00  118
 23  \w     77.00 103.00   0.50    0.10    --  106.08 -95.00-120.00   52
 24  \w     83.00 112.00   0.50    0.10    --  106.08-125.00-180.00   58
 25  \w     73.00 107.00   0.50    0.10    --  106.08-125.00-150.00   68
 26  \w     44.00  69.00   0.50    0.10    --  106.08-125.00-150.00   50
 27  \w     52.00  77.00   0.50    0.05    --   46.98-125.00-180.00   50
 28  \w     36.00 102.00   0.50    0.10    --  106.08 -95.00-150.00  132
 29  \w     77.00 103.00   0.50    0.10    --  106.08 -95.00 -30.00   52
 30  \w     37.00  75.00   0.50    0.10    --  106.08 -95.00 -30.00   76
 31  \w     34.00  64.00   0.50    0.10    --  106.08 -95.00  30.00   60
 32  \w     68.00 103.00   0.50    0.10    --  106.08 -95.00  30.00   70
 33  \w    -91.00 -44.00   0.50    0.05    --  -46.98 125.00 120.00   94
 34  \w    -93.00 -49.00   0.50    0.10    -- -103.00 125.00-150.00   88
 35  \w   -115.00 -35.00   0.50    0.05    --  -46.98 -47.00 159.00  160
 36  \w   -173.00 -90.00   0.50    0.10    -- -103.00 -47.00 159.00  166
;
_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      0.1820812000
_diffrn_orient_matrix_UB_12      -0.1110844000
_diffrn_orient_matrix_UB_13      -0.0388717000
_diffrn_orient_matrix_UB_21      -0.1180320000
_diffrn_orient_matrix_UB_22      -0.0781567000
_diffrn_orient_matrix_UB_23      -0.0523714000
_diffrn_orient_matrix_UB_31      -0.0252284000
_diffrn_orient_matrix_UB_32      0.1622047000
_diffrn_orient_matrix_UB_33      -0.0917265000
_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  0.0512
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6947
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.744
_diffrn_reflns_theta_max         66.744
_diffrn_reflns_theta_min         3.229
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53054
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       prism
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1014P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2424
_reflns_number_total             2714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01463d2.cif
_cod_data_source_block           crys505a
_cod_depositor_comments
'Adding full bibliography for 7716793--7716795.cif.'
_cod_original_cell_volume        773.18(7)
_cod_database_code               7716794
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.513
_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), C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B), C13(H13A,
 H13B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C6(H6)
2.d Idealised tetrahedral OH refined as rotating group:
 O16(H16), O14(H14)
;
_shelx_res_checksum              46036
_olex2_submission_original_sample_id C-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 2.308
_oxdiff_exptl_absorpt_empirical_full_min 0.363