A dinuclear copper(II) complex with photoswitchable catechol oxidation activity.
Marcon, Michela; Crespi, Stefano; Pielmeier, Andreas; König, Burkhard; Chemical communications (Cambridge, England) 59 (2023) 948–951; doi:10.1039/d2cc06250j

data_7131141
_publ_section_title
;
 A dinuclear copper(II) complex with photoswitchable catechol oxidation
 activity.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              948
_journal_page_last               951
_journal_paper_doi               10.1039/d2cc06250j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C38 H36 Cl4 Cu2 N8, [+ solvents]'
_chemical_formula_sum            'C38 H36 Cl4 Cu2 N8'
_chemical_formula_weight         873.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-13
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-07 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1219(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.44092(4)
_cell_length_b                   11.74337(5)
_cell_length_c                   22.12241(10)
_cell_measurement_reflns_used    53742
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.5170
_cell_measurement_theta_min      3.9160
_cell_volume                     2414.499(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (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      123.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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     27.00  52.00   0.50    0.15    --   20.00  75.00 -30.56   50
  2  \w     41.00  66.00   0.50    0.15    --   36.00  77.00 -16.19   50
  3  \w     43.00  68.00   0.50    0.15    --   36.00  74.00 -31.31   50
  4  \w     44.00  69.00   0.50    0.15    --   36.00  73.00 -37.98   50
  5  \w     30.00  55.00   0.50    0.15    --   24.00  76.00 -61.61   50
  6  \w     29.00  54.00   0.50    0.15    --   24.00  77.00 -88.86   50
  7  \w     38.00  63.00   0.50    0.15    --   32.00  76.00-121.78   50
  8  \w     48.00  73.00   0.50    0.15    --   40.00  73.00 -84.67   50
  9  \w     56.00  81.00   0.50    0.15    --   48.00  72.00-101.13   50
 10  \w     44.00  69.00   0.50    0.15    --   36.00  73.00 -62.71   50
 11  \w     54.00  79.00   0.50    0.15    --   44.00  70.00 -88.64   50
 12  \w     44.00  69.00   0.50    0.15    --   36.00  72.00 -46.07   50
 13  \w     44.00  69.00   0.50    0.15    --   36.00  72.00 -21.65   50
 14  \w     48.00  73.00   0.50    0.15    --   40.00  72.00 -12.05   50
 15  \w     57.00  82.00   0.50    0.15    --   48.00  71.00   2.91   50
 16  \w     58.00  83.00   0.50    0.15    --   48.00  67.00 -11.33   50
 17  \w     58.00  83.00   0.50    0.15    --   48.00  68.00 -90.77   50
 18  \w     60.00  85.00   0.50    0.15    --   48.00  60.00 -57.02   50
 19  \w     51.00  76.00   0.50    0.15    --   40.00  62.00 -36.97   50
 20  \w     56.00  81.00   0.50    0.15    --   44.00  60.00 -26.46   50
 21  \w     56.00  81.00   0.50    0.15    --   44.00  61.00 -17.47   50
 22  \w    -56.00 -31.00   0.50    0.15    --  -72.00  51.00-138.09   50
 23  \w    -84.00 -31.00   0.50    0.15    --  -66.64 125.00 -30.00  106
 24  \w    -24.00   1.00   0.50    0.15    --  -24.00  86.00 -35.26   50
 25  \w     84.00 110.00   0.50    0.15    --   77.25  78.00 -17.40   52
 26  \w     75.00 100.00   0.50    0.15    --   68.00  75.00 -70.04   50
 27  \w     72.00  97.00   0.50    0.15    --   64.00  73.00 -73.12   50
 28  \w     68.00  93.00   0.50    0.15    --   60.00  72.00 -66.05   50
 29  \w     74.00  99.00   0.50    0.15    --   68.00  76.00 -94.31   50
 30  \w     68.00  93.00   0.50    0.15    --   60.00  72.00-123.28   50
 31  \w     75.00 100.00   0.50    0.15    --   68.00  75.00-134.09   50
 32  \w     66.00  91.00   0.50    0.15    --   56.00  70.00-112.27   50
 33  \w     70.00  95.00   0.50    0.15    --   60.00  70.00-114.50   50
 34  \w     88.00 113.00   0.50    0.15    --   77.25  65.00-147.68   50
 35  \w     88.00 113.00   0.50    0.15    --   77.25  66.00-105.40   50
 36  \w     88.00 113.00   0.50    0.15    --   77.25  64.00-173.57   50
 37  \w     88.00 113.00   0.50    0.15    --   77.25  65.00 -95.58   50
 38  \w     88.00 113.00   0.50    0.15    --   77.25  65.00 -80.81   50
 39  \w     67.00  92.00   0.50    0.15    --   56.00  62.00 -90.47   50
 40  \w     64.00  89.00   0.50    0.15    --   52.00  60.00 -71.69   50
 41  \w     68.00  93.00   0.50    0.15    --   56.00  61.00  -9.16   50
 42  \w     67.00  92.00   0.50    0.15    --   56.00  62.00  -5.25   50
 43  \w     64.00  89.00   0.50    0.15    --   56.00  72.00   1.11   50
 44  \w     68.00  93.00   0.50    0.15    --   56.00  59.00 -21.97   50
 45  \w     92.00 117.00   0.50    0.15    --   77.25  54.00-110.67   50
 46  \w     93.00 118.00   0.50    0.15    --   77.25  40.00-126.62   50
 47  \w     68.00  93.00   0.50    0.15    --   56.00  59.00 -74.05   50
 48  \w     93.00 118.00   0.50    0.15    --   77.25  39.00-147.34   50
 49  \w     92.00 117.00   0.50    0.15    --   77.25  38.00 -61.87   50
 50  \w     96.00 122.00   0.50    0.15    --   77.25  39.00 -46.66   52
 51  \w     89.00 121.00   0.50    0.15    --   77.25  36.00 -13.92   64
 52  \w     92.00 119.00   0.50    0.15    --   77.25  38.00  83.72   54
 53  \w     79.00 105.00   0.50    0.15    --   77.25  26.00 131.19   52
 54  \w     90.00 119.00   0.50    0.15    --   77.25  53.00  43.74   58
 55  \w     64.00  89.00   0.50    0.15    --   52.00  58.00 -18.84   50
 56  \w     92.00 119.00   0.50    0.15    --   76.72  15.00-150.00   54
 57  \w     52.00  77.00   0.50    0.15    --   76.72  15.00-150.00   50
 58  \w     60.00  86.00   0.50    0.15    --   76.72  19.00-163.00   52
 59  \w     61.00  86.00   0.50    0.15    --   72.87  19.00-163.00   50
 60  \w     42.00  91.00   0.50    0.15    --   76.72   0.00-150.00   98
 61  \w     47.00 103.00   0.50    0.15    --   64.77  19.00-163.00  112
 62  \w     71.00 113.00   0.50    0.15    --   76.72  15.00 -30.00   84
 63  \w     58.00 102.00   0.50    0.15    --   76.72   0.00 -30.00   88
 64  \w     68.00 111.00   0.50    0.15    --   76.72  15.00  30.00   86
 65  \w     40.00  74.00   0.50    0.15    --   77.25  -3.00  49.37   68
 66  \w     51.00  81.00   0.50    0.15    --   77.25  -4.00 111.03   60
 67  \w     -5.00  20.00   0.50    0.15    --    4.00  99.00-112.80   50
 68  \w     40.00  71.00   0.50    0.15    --   77.25  -4.00 -97.84   62
 69  \w     37.00  65.00   0.50    0.15    --   77.25 -57.00-158.71   56
 70  \w     26.00  73.00   0.50    0.15    --   64.77-125.00 -30.00   94
 71  \w     23.00  79.00   0.50    0.15    --   64.77-125.00  90.00  112
 72  \w     38.00  63.00   0.50    0.15    --   76.72-125.00  90.00   50
 73  \w     55.00  96.00   0.50    0.15    --   76.72-125.00 120.00   82
 74  \w     27.00  90.00   0.50    0.15    --   64.77-125.00   0.00  126
 75  \w     58.00  84.00   0.50    0.15    --   72.87-125.00 -30.00   52
 76  \w     36.00  62.00   0.50    0.15    --   64.77-125.00-150.00   52
 77  \w     43.00  88.00   0.50    0.15    --   76.72-125.00 -90.00   90
 78  \w     55.00 103.00   0.50    0.15    --   76.72-125.00 -60.00   96
 79  \w     46.00 103.00   0.50    0.15    --   76.72-125.00-120.00  114
 80  \w     39.00 103.00   0.50    0.15    --   76.72-125.00 -30.00  128
 81  \w     42.00 103.00   0.50    0.15    --   76.72-125.00   0.00  122
 82  \w     46.00 100.00   0.50    0.15    --   76.72-125.00  60.00  108
 83  \w     39.00  83.00   0.50    0.15    --   77.25-120.00 121.27   88
 84  \w     35.00  60.00   0.50    0.15    --   76.72-125.00 150.00   50
 85  \w     51.00  76.00   0.50    0.15    --   77.25 -92.00 134.33   50
 86  \w     35.00  72.00   0.50    0.15    --   77.25-120.00  99.92   74
 87  \w     44.00 101.00   0.50    0.15    --   77.25-119.00  24.00  114
 88  \w     40.00  75.00   0.50    0.15    --   77.25-104.00 -37.51   70
 89  \w    -84.00 -59.00   0.50    0.15    --  -48.00 -69.00 -43.98   50
 90  \w    -84.00 -58.00   0.50    0.15    --  -48.00 -70.00 -38.83   52
 91  \w    -76.00 -51.00   0.50    0.15    --  -40.00 -70.00 -92.14   50
 92  \w    -80.00 -55.00   0.50    0.15    --  -44.00 -71.00-127.00   50
 93  \w    -74.00 -48.00   0.50    0.15    --  -40.00 -72.00-109.87   52
 94  \w   -106.00 -81.00   0.50    0.15    --  -73.25 -77.00 -23.38   50
 95  \w   -105.00 -79.00   0.50    0.15    --  -73.25 -76.00   0.90   52
 96  \w   -106.00 -81.00   0.50    0.15    --  -73.25 -77.00 -52.31   50
 97  \w   -105.00 -79.00   0.50    0.15    --  -72.00 -76.00 -62.41   52
 98  \w   -104.00 -78.00   0.50    0.15    --  -72.00 -76.00 -35.80   52
 99  \w   -105.00 -79.00   0.50    0.15    --  -73.25 -76.00 -42.77   52
100  \w   -105.00 -79.00   0.50    0.15    --  -73.25 -76.00 -75.25   52
101  \w   -104.00 -78.00   0.50    0.15    --  -72.00 -76.00 -39.98   52
102  \w   -107.00 -80.00   0.50    0.15    --  -73.25 -76.00 -49.27   54
103  \w   -107.00 -80.00   0.50    0.15    --  -73.25 -75.00 -46.11   54
104  \w   -106.00 -79.00   0.50    0.15    --  -73.25 -76.00 -98.35   54
105  \w   -104.00 -78.00   0.50    0.15    --  -73.25 -77.00-127.06   52
106  \w   -105.00 -79.00   0.50    0.15    --  -73.25 -76.00-122.83   52
107  \w   -107.00 -80.00   0.50    0.15    --  -73.25 -74.00-113.60   54
108  \w   -107.00 -82.00   0.50    0.15    --  -73.25 -75.00-104.46   50
109  \w   -109.00 -84.00   0.50    0.15    --  -73.25 -71.00 -95.67   50
110  \w    -98.00 -72.00   0.50    0.15    --  -64.00 -72.00 -67.33   52
111  \w    -98.00 -73.00   0.50    0.15    --  -64.00 -71.00 -17.46   50
112  \w   -105.00 -80.00   0.50    0.15    --  -73.25 -75.00 -19.34   50
113  \w    -92.00 -67.00   0.50    0.15    --  -56.00 -70.00 -18.81   50
114  \w   -106.00 -80.00   0.50    0.15    --  -72.00 -73.00 -15.79   52
115  \w    -96.00 -71.00   0.50    0.15    --  -60.00 -70.00-126.60   50
116  \w   -104.00 -79.00   0.50    0.15    --  -64.00 -58.00-109.91   50
117  \w   -108.00 -47.00   0.50    0.15    --  -66.64 -19.00  29.00  122
118  \w    -76.00 -50.00   0.50    0.15    --  -67.59 -19.00  29.00   52
119  \w   -109.00 -84.00   0.50    0.15    --  -73.25 -70.00 173.55   50
120  \w   -109.00 -84.00   0.50    0.15    --  -68.00 -55.00  23.54   50
121  \w   -106.00 -66.00   0.50    0.15    --  -73.25-145.00 -85.07   80
122  \w   -106.00 -80.00   0.50    0.15    --  -73.25 -89.00 -94.94   52
123  \w   -107.00 -81.00   0.50    0.15    --  -73.25 -88.00-121.60   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1550749000
_diffrn_orient_matrix_UB_12      -0.0132722000
_diffrn_orient_matrix_UB_13      -0.0352047000
_diffrn_orient_matrix_UB_21      0.0511271000
_diffrn_orient_matrix_UB_22      0.0306810000
_diffrn_orient_matrix_UB_23      -0.0603746000
_diffrn_orient_matrix_UB_31      0.0286204000
_diffrn_orient_matrix_UB_32      -0.1268550000
_diffrn_orient_matrix_UB_33      -0.0108918000
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            76090
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.994
_diffrn_reflns_theta_min         4.060
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.373
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.83a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0579P)^2^+1.3289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4851
_reflns_number_total             4956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06250j2.cif
_cod_data_source_block           u105
_cod_depositor_comments          'Adding full bibliography for 7131141.cif.'
_cod_original_cell_volume        2414.498(18)
_cod_database_code               7131141
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H36 Cl4 Cu2 N8'
_chemical_oxdiff_usercomment     Marcon_Koenig_mm239
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.511
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00C(H00C,H00D), C00D(H00E,H00F)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00G), C00H(H00I), C00O(H00P), C00Q(H00R)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 176 electrons were 
found in a volume of 790\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H10O] per Asymmetric Unit which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88014
_shelx_hkl_checksum              34931
_shelx_fab_checksum              41153
_olex2_date_sample_data_collection 2021-10-05
_olex2_date_sample_submission    2021-10-04
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems CryoStream 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with inert oil'
_olex2_submission_original_sample_id mm239
_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 1.474
_oxdiff_exptl_absorpt_empirical_full_min 0.793