Synthesis and characterization of a novel copper carboxylate complex and a copper complex-coated polyether sulfone membrane for efficient degradation of methylene blue dye under UV irradiation: the single crystal X-ray structure of the copper carboxylate complex.
Dhir, Rupy; Shah, Bulle; Singh, Narinder; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9441–9451; doi:10.1039/d4dt00871e

data_7716019
_publ_section_title
;
 Synthesis and characterization of a novel copper carboxylate complex and
 a copper complex-coated polyether sulfone membrane for efficient
 degradation of methylene blue dye under UV irradiation: the single
 crystal X-ray structure of the copper carboxylate complex.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9441
_journal_page_last               9451
_journal_paper_doi               10.1039/d4dt00871e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H28 Cu4 N4 O8, 2(Br), Cu H4 N2 O9, 2(H)'
_chemical_formula_sum            'C28 H34 Br2 Cu5 N6 O17'
_chemical_formula_weight         1204.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-12
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_audit_update_record
;
2023-03-05 deposited with the CCDC.	2024-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.766(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0204(5)
_cell_length_b                   16.7422(5)
_cell_length_c                   14.6331(4)
_cell_measurement_reflns_used    6091
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1690
_cell_measurement_theta_min      3.4100
_cell_volume                     4167.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.928
_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    -43.00   9.00   0.50    7.10    --   -9.95 102.00 175.00  104
  2  \w    -13.00  38.00   0.50    7.10    --   10.22-102.00  72.00  102
  3  \w    -52.00 -13.00   0.50    7.10    --   -9.95 125.00 -60.00   78
  4  \w    -71.00   3.00   0.50    7.10    --   -9.95 -38.00  90.00  148
  5  \w    -28.00  -3.00   0.50    7.10    --   -9.95 125.00  30.00   50
  6  \w    -56.00 -22.00   0.50    7.10    --   -9.95 125.00 120.00   68
  7  \w    -66.00 -14.00   0.50    7.10    --   -9.95 -38.00-120.00  104
  8  \w     37.00  74.00   0.50    7.10    --   10.22  38.00  30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0223614000
_diffrn_orient_matrix_UB_12      -0.0340780000
_diffrn_orient_matrix_UB_13      0.0116021000
_diffrn_orient_matrix_UB_21      0.0330832000
_diffrn_orient_matrix_UB_22      -0.0159499000
_diffrn_orient_matrix_UB_23      0.0243702000
_diffrn_orient_matrix_UB_31      -0.0120076000
_diffrn_orient_matrix_UB_32      0.0194748000
_diffrn_orient_matrix_UB_33      0.0402827000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14152
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.411
_diffrn_reflns_theta_min         3.236
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.502
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_F_000             2380
_refine_diff_density_max         3.066
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.373
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+37.2301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3218
_reflns_number_total             4561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00871e1.cif
_cod_data_source_block           pat-dicu
_cod_depositor_comments          'Adding full bibliography for 7716019.cif.'
_cod_original_cell_volume        4167.85(19)
_cod_database_code               7716019
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O Cu'
_diffrn_oxdiff_ac3_digest_frames
;
0118310156d3437e374dd02b499b67dbb4007286778
;
_diffrn_oxdiff_ac3_digest_hkl
;
012ad26fb44a1a9ac1e3591a4a292e17d44d17
;
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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,H) groups
2. Others
 Fixed Sof: H5AB(0.5) H5AC(0.5) H6AB(0.5) H6AC(0.5) H(0.5) HA(0.5)
3.a Rotating group:
 O5AA(H5AB,H5AC), O6AA(H6AB,H6AC), O9AA(H,HA)
3.b Secondary CH2 refined with riding coordinates:
 C3AA(H3AA,H3AB), C4AA(H4AA,H4AB)
3.c Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C0AA(H0AA), C1AA(H1AA), C5AA(H5AA), C6AA(H6AA), C7AA(H7AA),
 C8AA(H8AA), C9AA(H9AA), C0BA(H0BA), C1BA(H1BA)
;
_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 1.629
_oxdiff_exptl_absorpt_empirical_full_min 0.781