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_7046800
_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         'C30 H56 Cl2 Cu2 N14, 2(F6 Sb)'
_chemical_formula_sum            'C30 H56 Cl2 Cu2 F12 N14 Sb2'
_chemical_formula_weight         1282.36
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                hi_az16
_audit_creation_date             2016-09-21
_audit_creation_method
;
Olex2 1.2
(compiled Sep  9 2016 16:03:45 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.08984(16)
_cell_length_b                   18.88601(13)
_cell_length_c                   15.90472(14)
_cell_measurement_reflns_used    47362
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.3700
_cell_measurement_theta_min      3.5440
_cell_volume                     4833.01(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      perfluoro
_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 0.998
_diffrn_measured_fraction_theta_max 0.985
_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    -42.00  48.00   0.50   12.50    --   27.02 -57.00 -30.00  180
  2  \w     -3.00  97.00   0.50   12.50    --   27.02  77.00 -90.00  200
  3  \w      7.00  96.00   0.50   12.50    --   27.02  57.00-150.00  178
  4  \w      7.00  96.00   0.50   12.50    --   27.02  57.00  30.00  178
  5  \w     12.00  96.00   0.50   12.50    --   27.02-144.00 -22.00  168
  6  \w    -43.00  57.00   0.50   12.50    --   27.02 -77.00 150.00  200
  7  \w    -42.00  48.00   0.50   12.50    --   27.02 -57.00-120.00  180
  8  \w    -20.00  69.00   0.50   12.50    --   27.02 -99.00  60.00  178
  9  \w     -3.00  97.00   0.50   12.50    --   27.02  77.00  90.00  200
 10  \w      2.00  99.00   0.50   12.50    --   27.02  38.00  30.00  194
 11  \w     -3.00  97.00   0.50   12.50    --   27.02  77.00 120.00  200
 12  \w     -3.00  97.00   0.50   12.50    --   27.02  77.00   0.00  200
 13  \w    -20.00  69.00   0.50   12.50    --   27.02 -99.00-150.00  178
 14  \w     -3.00  97.00   0.50   12.50    --   27.02  77.00-180.00  200
 15  \w      2.00  81.00   0.50   12.50    --   27.02  38.00-150.00  158
 16  \w    -42.00  48.00   0.50   12.50    --   27.02 -57.00  60.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  '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      -0.0023225000
_diffrn_orient_matrix_UB_12      0.0373479000
_diffrn_orient_matrix_UB_13      0.0041584000
_diffrn_orient_matrix_UB_21      0.0414985000
_diffrn_orient_matrix_UB_22      0.0030313000
_diffrn_orient_matrix_UB_23      -0.0146146000
_diffrn_orient_matrix_UB_31      -0.0147184000
_diffrn_orient_matrix_UB_32      0.0026282000
_diffrn_orient_matrix_UB_33      -0.0419118000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            174732
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.421
_diffrn_reflns_theta_min         3.036
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.171
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.097
_refine_diff_density_max         3.079
_refine_diff_density_min         -2.506
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         8562
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+14.5636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7213
_reflns_number_total             8562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01234b2.cif
_cod_data_source_block           hi_az16
_cod_depositor_comments
'Adding full bibliography for 7046798--7046801.cif.'
_cod_database_code               7046800
_audit_block_refno               2765
_audit_block_usercomment         'hi_az307a, block, black'
_chemical_oxdiff_formula         'C30 H56 F12 N14 Cu2 Cl2 Sb2'
_chemical_oxdiff_usercomment     'hi_az307a, block, black'
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.812
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sb1-F11 \\sim Sb1-F12 \\sim Sb1-F13 \\sim Sb1-F14 \\sim Sb2-F21 \\sim Sb2-F22
\\sim Sb2-F23 \\sim Sb2-F24
 with sigma of 0.02
 F11-F12 \\sim F11-F13 \\sim F14-F12 \\sim F14-F13 \\sim F12-F13 \\sim
F12-F13_$1 \\sim F21-F22 \\sim F21-
 F23 \\sim F24-F22 \\sim F24-F23 \\sim F22-F23 \\sim F22-F23_$2
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Sb2, Sb1, F11, F13, F14, F21, F12, F22, F23, F24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              52805
_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 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.915
_cell_oxdiff_length_a            16.08665(16)
_cell_oxdiff_length_b            18.8831(2)
_cell_oxdiff_length_c            15.9103(2)
_cell_oxdiff_angle_alpha         90.0294(11)
_cell_oxdiff_angle_beta          90.0212(11)
_cell_oxdiff_angle_gamma         90.0129(10)
_cell_oxdiff_volume              4833.01(11)
_cell_oxdiff_measurement_reflns_used 47362