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_7716795
_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         'C30 H46 Cu2 N2 O12, 2(H2 O)'
_chemical_formula_sum            'C30 H50 Cu2 N2 O14'
_chemical_formula_weight         789.80
_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             2023-03-14
_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                85.818(3)
_cell_angle_beta                 75.310(3)
_cell_angle_gamma                88.591(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1604(3)
_cell_length_b                   12.2855(4)
_cell_length_c                   15.6941(6)
_cell_measurement_reflns_used    8949
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      66.5700
_cell_measurement_theta_min      4.4730
_cell_volume                     1703.90(10)
_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      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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -70.00 -41.00   0.50    0.05    -- -103.00  61.00-120.00   58
  2  \w    -66.00 -37.00   0.50    0.05    -- -103.00  61.00 -90.00   58
  3  \w    -69.00 -36.00   0.50    0.05    -- -103.00  61.00 -30.00   66
  4  \w    -70.00 -31.00   0.50    0.05    -- -103.00  61.00   0.00   78
  5  \w    -70.00 -33.00   0.50    0.05    -- -103.00  61.00  30.00   74
  6  \w    -70.00 -45.00   0.50    0.05    -- -103.00  61.00 150.00   50
  7  \w    -70.00 -45.00   0.50    0.05    -- -103.00  61.00  60.00   50
  8  \w    -70.00 -35.00   0.50    0.05    -- -103.00  61.00-180.00   70
  9  \w    -16.00  26.00   0.50    0.05    --  -47.23  19.00-120.00   84
 10  \w    -13.00  17.00   0.50    0.05    --  -47.23  19.00-150.00   60
 11  \w   -101.00 -73.00   0.50    0.05    --  -47.23   0.00 -90.00   56
 12  \w    -82.00   1.00   0.50    0.05    --  -47.23 107.00  55.00  166
 13  \w    -65.00 -39.00   0.50    0.05    -- -103.00 107.00  55.00   52
 14  \w   -104.00 -33.00   0.50    0.05    -- -103.00 125.00  30.00  142
 15  \w   -103.00 -77.00   0.50    0.05    -- -103.00 107.00  55.00   52
 16  \w   -164.00 -95.00   0.50    0.05    -- -103.00 -45.00 -90.00  138
 17  \w   -112.00 -83.00   0.50    0.05    --  -47.23 -38.00   0.00   58
 18  \w    -82.00 -56.00   0.50    0.05    --  -47.23 -38.00   0.00   52
 19  \w   -115.00 -90.00   0.50    0.05    -- -103.00 -45.00  30.00   50
 20  \w   -168.00-127.00   0.50    0.05    -- -103.00 -45.00  30.00   82
 21  \w   -127.00 -87.00   0.50    0.05    -- -103.00-107.00 -42.00   80
 22  \w    -25.00   1.00   0.50    0.05    --   47.23 -19.00  90.00   52
 23  \w    -26.00  15.00   0.50    0.05    --   47.23 -19.00  30.00   82
 24  \w    -13.00  57.00   0.50    0.05    --   47.23 -57.00   0.00  140
 25  \w    124.00 154.00   0.50    0.05    --  106.08 107.00  55.00   60
 26  \w    -23.00  22.00   0.50    0.05    --   47.23 -19.00-120.00   90
 27  \w     57.00  96.00   0.50    0.05    --  106.08-125.00 -60.00   78
 28  \w     68.00  93.00   0.50    0.05    --  106.08-107.00 -42.00   50
 29  \w     43.00 101.00   0.50    0.05    --  106.08-125.00-120.00  116
 30  \w     57.00 104.00   0.50    0.05    --  106.08 -95.00-150.00   94
 31  \w      9.00  35.00   0.50    0.05    --   47.23-107.00 -42.00   52
 32  \w     77.00 102.00   0.50    0.05    --  106.08 -95.00 -30.00   50
 33  \w     45.00 112.00   0.50    0.05    --  106.08-125.00 150.00  134
 34  \w    109.00 178.00   0.50    0.05    --  106.08   0.00 150.00  138
 35  \w    140.00 178.00   0.50    0.05    --  106.08  30.00 150.00   76
 36  \w     99.00 124.00   0.50    0.05    --  106.08  30.00 150.00   50
 37  \w    109.00 159.00   0.50    0.05    --  106.08   0.00  60.00  100
 38  \w    152.00 177.00   0.50    0.05    --  106.08  45.00  30.00   50
 39  \w     98.00 124.00   0.50    0.05    --  106.08  45.00  30.00   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      0.0074741000
_diffrn_orient_matrix_UB_12      0.0190936000
_diffrn_orient_matrix_UB_13      -0.0991239000
_diffrn_orient_matrix_UB_21      0.0061443000
_diffrn_orient_matrix_UB_22      -0.1242450000
_diffrn_orient_matrix_UB_23      -0.0086071000
_diffrn_orient_matrix_UB_31      -0.1735932000
_diffrn_orient_matrix_UB_32      -0.0027797000
_diffrn_orient_matrix_UB_33      0.0211559000
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16867
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.679
_diffrn_reflns_theta_max         66.679
_diffrn_reflns_theta_min         3.607
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29415
_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    1.539
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.583
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1301P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4737
_reflns_number_total             5933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01463d2.cif
_cod_data_source_block           crys506a
_cod_depositor_comments
'Adding full bibliography for 7716793--7716795.cif.'
_cod_database_code               7716795
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.686
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Secondary CH2 refined with riding coordinates:
 C14B(H14A,H14B), C15B(H15A,H15B), C15A(H15C,H15D), C14A(H14C,H14D), C10A(H10A,
 H10B), C12B(H12A,H12B), C10B(H10C,H10D), C13A(H13A,H13B), C12A(H12C,H12D),
 C13B(H13C,H13D), C6A(H6AA,H6AB), C11A(H11A,H11B), C6B(H6BA,H6BB), C11B(H11C,
 H11D)
2.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C9A(H9A), C4A(H4A), C4B(H4B), C9B(H9B), C8A(H8A), C8B(H8B)
2.d Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
2.e Idealised tetrahedral OH refined as rotating group:
 O2B(H2B), O6A(H6A), O2A(H2A), O6B(H6B)
;
_shelx_res_checksum              61454
_olex2_submission_original_sample_id D-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 2.138
_oxdiff_exptl_absorpt_empirical_full_min 0.343