Intramolecular metal-ligand electron transfer triggered by co-ligand substitution.
Ziesak, Alexandra; Steuer, Lena; Kaifer, Elisabeth; Wagner, Norbert; Beck, Johannes; Wadepohl, Hubert; Himmel, Hans-Jörg; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9430–9441; doi:10.1039/c8dt01234b

data_7046801
_publ_section_title
;
 Intramolecular metal-ligand electron transfer triggered by co-ligand
 substitution.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9430
_journal_page_last               9441
_journal_paper_doi               10.1039/c8dt01234b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C18 H24 Cu N6, C6 H8 N2, H2 O, 2(Cl)'
_chemical_formula_sum            'C24 H34 Cl2 Cu N8 O'
_chemical_formula_weight         585.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                hi_az20
_audit_creation_date             2017-03-16
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                69.734(4)
_cell_angle_beta                 89.956(3)
_cell_angle_gamma                82.315(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6115(4)
_cell_length_b                   11.2052(4)
_cell_length_c                   12.3212(6)
_cell_measurement_reflns_used    13466
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.5170
_cell_measurement_theta_min      4.2170
_cell_volume                     1360.37(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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    -21.00  69.00   1.00    2.00    --    0.00  57.00  90.00   90
  2  \w    -26.00  72.00   1.00    2.00    --    0.00  38.00 -90.00   98
  3  \w    -26.00  72.00   1.00    2.00    --    0.00  38.00-150.00   98
  4  \w     36.00  85.00   1.00   16.00    --  108.00 -92.00-120.00   49
  5  \w    -35.00  10.00   1.00    2.00    --   14.00 111.00-145.76   45
  6  \w    -38.00 -11.00   1.00    8.00    --   30.00 142.00  -7.43   27
  7  \w     -9.00  18.00   1.00    8.00    --   34.00 102.00-142.50   27
  8  \w      5.00  32.00   1.00    8.00    --   42.00  90.00 -96.55   27
  9  \w     12.00  38.00   1.00    8.00    --   46.00  84.00-125.19   26
 10  \w     13.00  45.00   1.00    8.00    --   46.00  82.00 156.48   32
 11  \w     13.00  40.00   1.00    8.00    --   46.00  83.00 -28.63   27
 12  \w     12.00  38.00   1.00    8.00    --   46.00  84.00 115.66   26
 13  \w     12.00  38.00   1.00    8.00    --   46.00  84.00  48.46   26
 14  \w     26.00 123.00   1.00    8.00    --   54.00  73.00  20.50   97
 15  \w     24.00 124.00   1.00    8.00    --   54.00  77.00  90.00  100
 16  \w     24.00 124.00   1.00    8.00    --   54.00  77.00 120.00  100
 17  \w     24.00 124.00   1.00    8.00    --   54.00  77.00-180.00  100
 18  \w      1.00  96.00   1.00    8.00    --   54.00 -99.00   0.00   95
 19  \w     24.00 124.00   1.00    8.00    --   54.00  77.00  30.00  100
 20  \w     24.00 124.00   1.00    8.00    --   54.00  77.00 -90.00  100
 21  \w     24.00 124.00   1.00    8.00    --   54.00  77.00  60.00  100
 22  \w     33.00 123.00   1.00    8.00    --   54.00  57.00-120.00   90
 23  \w    -15.00  75.00   1.00    8.00    --   54.00 -57.00  30.00   90
 24  \w     25.00 124.00   1.00    8.00    --   54.00  75.00 -39.69   99
 25  \w     24.00 124.00   1.00    8.00    --   54.00  77.00 150.00  100
 26  \w     28.00 123.00   1.00    8.00    --   54.00  70.00-110.30   95
 27  \w      1.00  96.00   1.00    8.00    --   54.00 -99.00-180.00   95
 28  \w     23.00 111.00   1.00    8.00    --   54.00-125.00 -60.00   88
 29  \w     23.00  49.00   1.00    8.00    --   54.00  78.00-131.84   26
 30  \w     24.00 124.00   1.00    8.00    --   54.00  77.00   0.00  100
 31  \w     37.00 127.00   1.00    8.00    --   58.00  58.00   1.64   90
 32  \w     28.00 128.00   1.00    8.00    --   58.00  77.00-167.07  100
 33  \w     37.00 127.00   1.00    8.00    --   58.00  58.00  75.63   90
 34  \w     40.00 132.00   1.00    8.00    --   62.00  49.00   3.94   92
 35  \w     33.00 132.00   1.00    8.00    --   62.00  76.00 -59.27   99
 36  \w     42.00 138.00   1.00    8.00    --   66.00  43.00-134.33   96
 37  \w     44.00 136.00   1.00    8.00    --   66.00  51.00 -24.14   92
 38  \w     45.00 135.00   1.00    8.00    --   66.00  56.00-103.87   90
 39  \w     45.00 135.00   1.00    8.00    --   66.00  57.00 -31.04   90
 40  \w     37.00 136.00   1.00    8.00    --   66.00  75.00-104.96   99
 41  \w     44.00 136.00   1.00    8.00    --   66.00  50.00 160.07   92
 42  \w     45.00 135.00   1.00    8.00    --   66.00  54.00  36.51   90
 43  \w     43.00 139.00   1.00    8.00    --   70.00  71.00-109.32   96
 44  \w     49.00 139.00   1.00    8.00    --   70.00  54.00  78.88   90
 45  \w     49.00 139.00   1.00    8.00    --   70.00  54.00-147.95   90
 46  \w     44.00 142.00   1.00    8.00    --   70.00  38.00   1.51   98
 47  \w     52.00 142.00   1.00    8.00    --   74.00  63.00  88.02   90
 48  \w     53.00 144.00   1.00    8.00    --   74.00  53.00 -87.18   91
 49  \w     52.00 147.00   1.00    8.00    --   78.00  70.00 -15.81   95
 50  \w     57.00 148.00   1.00    8.00    --   78.00  52.00  56.69   91
 51  \w     61.00 158.00   1.00   16.00    --   86.00  40.00  48.89   97
 52  \w     63.00 157.00   1.00   16.00    --   86.00  47.00  73.86   94
 53  \w     68.00 158.00   1.00   16.00    --   90.00  63.00 135.85   90
 54  \w     62.00 160.00   1.00   16.00    --   90.00  74.00 -33.21   98
 55  \w     60.00 160.00   1.00   16.00    --   90.00  77.00-155.70  100
 56  \w     65.00 164.00   1.00   16.00    --   94.00  76.00-133.70   99
 57  \w     71.00 167.00   1.00   16.00    --   98.00  72.00 -84.07   96
 58  \w     68.00 168.00   1.00   16.00    --   98.00  77.00 -20.38  100
 59  \w     85.00 175.00   1.00   16.00    --  108.00  64.00 150.00   90
 60  \w     78.00 178.00   1.00   16.00    --  108.00  77.00  60.00  100
 61  \w     78.00 178.00   1.00   16.00    --  108.00  77.00 -60.00  100
 62  \w     36.00 145.00   1.00   16.00    --  108.00 -92.00-120.00  109
 63  \w    107.00 145.00   1.00   16.00    --  108.00 -92.00-120.00   38
 64  \w     78.00 105.00   1.00   16.00    --  108.00  77.00  30.00   27
 65  \w     83.00 112.00   1.00   16.00    --  108.00  38.00 120.00   29
 66  \w     83.00 130.00   1.00   16.00    --  108.00  38.00  90.00   47
 67  \w     85.00 156.00   1.00   16.00    --  108.00  38.00 -30.00   71
 68  \w     82.00 109.00   1.00   16.00    --  108.00  38.00 -60.00   27
 69  \w     87.00 114.00   1.00   16.00    --  108.00  50.00-180.00   27
 70  \w     39.00 111.00   1.00   16.00    --  108.00-111.00-150.00   72
 71  \w     85.00 175.00   1.00   16.00    --  108.00  64.00  30.00   90
 72  \w     61.00 101.00   1.00   16.00    --  108.00 -38.00-120.00   40
 73  \w     36.00 146.00   1.00   16.00    --  108.00 -92.00  30.00  110
 74  \w     82.00 158.00   1.00   16.00    --  108.00  77.00-120.00   76
 75  \w     79.00 116.00   1.00   16.00    --  108.00-111.00 -60.00   37
 76  \w     47.00  74.00   1.00   16.00    --  108.00-111.00 -60.00   27
 77  \w     85.00 112.00   1.00   16.00    --  108.00  64.00  90.00   27
 78  \w     86.00 111.00   1.00   16.00    --  108.00  64.00-180.00   25
 79  \w     86.00 111.00   1.00   16.00    --  108.00  65.00  -6.69   25
 80  \w     86.00 111.00   1.00   16.00    --  108.00  64.00 -60.00   25
 81  \w    100.00 175.00   1.00   16.00    --  108.00 111.00  60.00   75
 82  \w     87.00 112.00   1.00   16.00    --  108.00  64.00  60.00   25
 83  \w     87.00 173.00   1.00   16.00    --  108.00  64.00 120.00   86
 84  \w     97.00 124.00   1.00   16.00    --  108.00  50.00 150.00   27
 85  \w    112.00 177.00   1.00   16.00    --  108.00  77.00 -90.00   65
 86  \w     79.00 106.00   1.00   16.00    --  108.00  77.00 -90.00   27
 87  \w     85.00 112.00   1.00   16.00    --  108.00  64.00-120.00   27
 88  \w     82.00 177.00   1.00   16.00    --  108.00  77.00 -30.00   95
 89  \w     70.00 129.00   1.00   16.00    --  108.00 -64.00   0.00   59
 90  \w     78.00 177.00   1.00   16.00    --  108.00  77.00-150.00   99
 91  \w     78.00 104.00   1.00   16.00    --  108.00  77.00  90.00   26
 92  \w     78.00 154.00   1.00   16.00    --  108.00  77.00   0.00   76
 93  \w     83.00 110.00   1.00   16.00    --  108.00  77.00 120.00   27
 94  \w     78.00 170.00   1.00   16.00    --  108.00  77.00-180.00   92
 95  \w     91.00 118.00   1.00   16.00    --  108.00  77.00 150.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0071987000
_diffrn_orient_matrix_UB_12      -0.1402189000
_diffrn_orient_matrix_UB_13      0.0828420000
_diffrn_orient_matrix_UB_21      0.1291246000
_diffrn_orient_matrix_UB_22      0.0089214000
_diffrn_orient_matrix_UB_23      0.0515790000
_diffrn_orient_matrix_UB_31      -0.0691899000
_diffrn_orient_matrix_UB_32      0.0467168000
_diffrn_orient_matrix_UB_33      0.0910179000
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            42653
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.646
_diffrn_reflns_theta_min         3.829
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.208
_exptl_absorpt_correction_T_max  0.79302
_exptl_absorpt_correction_T_min  0.78356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   1.304
_exptl_transmission_factor_min   0.827
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0674P)^2^+2.7305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4275
_reflns_number_total             5175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01234b2.cif
_cod_data_source_block           hi_az20
_cod_depositor_comments
'Adding full bibliography for 7046798--7046801.cif.'
_cod_original_cell_volume        1360.36(10)
_cod_database_code               7046801
_audit_block_refno               2841
_audit_block_usercomment         'hi_az336, block, blue'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 N7, N8, C19, C20, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Riding coordinates:
 N8(H8A,H8B), O1(H1A,H1B)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N6(H6A,H6B), C6(H6C,H6D), C12(H12A,H12B), C18(H18A,
 H18B), C24(H24A,H24B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.827
_shelx_res_checksum              84017
_cell_oxdiff_length_a            10.6115(4)
_cell_oxdiff_length_b            11.2052(4)
_cell_oxdiff_length_c            12.3212(6)
_cell_oxdiff_angle_alpha         69.734(4)
_cell_oxdiff_angle_beta          89.956(3)
_cell_oxdiff_angle_gamma         82.315(3)
_cell_oxdiff_volume              1360.36(9)
_cell_oxdiff_measurement_reflns_used 13466