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_7046799
_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
'0.5(C52 H100 Cl4 Cu4 N24), 2(C7 H5 N), 2(F6 Sb)'
_chemical_formula_sum            'C40 H60 Cl2 Cu2 F12 N14 Sb2'
_chemical_formula_weight         1406.50
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                hi_az19
_audit_creation_date             2017-01-31
_audit_creation_method
;
Olex2 1.2
(compiled Dec 12 2016 15:58:59 for OlexSys, GUI svn.r5292)
;
_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                   11.12549(13)
_cell_length_b                   22.2307(3)
_cell_length_c                   21.9849(3)
_cell_measurement_reflns_used    33531
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.7510
_cell_measurement_theta_min      3.1730
_cell_volume                     5437.47(12)
_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, 2009-17); 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 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -45.00  53.00   0.50   25.00    --   27.02 -38.00 -90.00  196
  2  \w    -20.00  69.00   0.50   25.00    --   27.02 -99.00  60.00  178
  3  \w      7.00  96.00   0.50   25.00    --   27.02  57.00   0.00  178
  4  \w     10.00  93.00   0.50   25.00    --   27.02-138.00 -29.00  166
  5  \w    -42.00  48.00   0.50   25.00    --   27.02 -57.00-150.00  180
  6  \w     -3.00  97.00   0.50   25.00    --   27.02  77.00-180.00  200
  7  \w    -42.00  48.00   0.50   25.00    --   27.02 -57.00 120.00  180
  8  \w     -3.00  97.00   0.50   25.00    --   27.02  77.00  60.00  200
  9  \w      7.00  96.00   0.50   25.00    --   27.02  57.00 -60.00  178
 10  \w    -49.00 -18.00   0.50   25.00    --    4.00 118.00 145.18   62
 11  \w     -4.00  25.00   0.50   25.00    --   27.02  79.00 -98.53   58
 12  \w      7.00  96.00   0.50   25.00    --   27.02  57.00 150.00  178
 13  \w    -20.00  69.00   0.50   25.00    --   27.02 -99.00-180.00  178
 14  \w     -5.00  24.00   0.50   25.00    --   27.02  80.00  32.15   58
 15  \w      7.00  96.00   0.50   25.00    --   27.02  57.00-150.00  178
 16  \w    -42.00  48.00   0.50   25.00    --   27.02 -57.00  60.00  180
 17  \w      7.00  86.00   0.50   25.00    --   27.02  57.00 -90.00  158
;
_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      0.0001936000
_diffrn_orient_matrix_UB_12      -0.0318889000
_diffrn_orient_matrix_UB_13      -0.0013261000
_diffrn_orient_matrix_UB_21      0.0389740000
_diffrn_orient_matrix_UB_22      -0.0009807000
_diffrn_orient_matrix_UB_23      0.0255105000
_diffrn_orient_matrix_UB_31      -0.0504532000
_diffrn_orient_matrix_UB_32      -0.0008646000
_diffrn_orient_matrix_UB_33      0.0196928000
_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  0.0706
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            176887
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.436
_diffrn_reflns_theta_min         2.605
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.938
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.787
_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 (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       plate
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         9622
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+5.7256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7473
_reflns_number_total             9622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01234b2.cif
_cod_data_source_block           hi_az19
_cod_depositor_comments
'Adding full bibliography for 7046798--7046801.cif.'
_cod_original_cell_volume        5437.48(11)
_cod_database_code               7046799
_audit_block_refno               2812
_chemical_oxdiff_formula         'C40 H60 Cl2 Cu2 F12 N14 Sb2'
_chemical_oxdiff_usercomment     'hi_az327a, plate, dark yellow'
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.760
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_shelxl_version_number           2016/6
_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
 Sb-F1 \\sim Sb-F2 \\sim Sb-F3 \\sim Sb-F4 \\sim Sb-F5 \\sim Sb-F6
 with sigma of 0.01
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F1-F5 \\sim F6-F2 \\sim F6-F3 \\sim F6-F4
\\sim F6-F5 \\sim F2-F3 \\sim F2-F5
 \\sim F3-F4 \\sim F4-F5
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F1, F2, F3, F4, F5, F6, Sb
 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:
 C2(H2), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
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)
;
_audit_block_usercomment         'hi_az327a, plate, dark yellow'
_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 1.189
_oxdiff_exptl_absorpt_empirical_full_min 0.864
_shelx_res_checksum              56133
_cell_oxdiff_length_a            11.12566(16)
_cell_oxdiff_length_b            22.2244(5)
_cell_oxdiff_length_c            21.9908(3)
_cell_oxdiff_angle_alpha         90.0135(14)
_cell_oxdiff_angle_beta          90.0118(12)
_cell_oxdiff_angle_gamma         89.9772(14)
_cell_oxdiff_volume              5437.48(16)
_cell_oxdiff_measurement_reflns_used 33535