Tuning of the Properties of Transition-Metal Bispidine Complexes by Variation of the Basicity of the Aromatic Donor Groups
Peter Comba; Michael Morgen; Hubert Wadepohl; Inorganic Chemistry 52 (2013) 6481–6501; doi:10.1021/ic4004214

data_4335061
_publ_section_title
;
 Tuning of the Properties of Transition-Metal Bispidine Complexes by
 Variation of the Basicity of the Aromatic Donor Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6481
_journal_page_last               6501
_journal_paper_doi               10.1021/ic4004214
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C27 H32 Cl4 Cu N6 O13'
_chemical_formula_weight         853.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mimo67
_audit_creation_date
;
'Mon Nov 19 15:51:56 2012'
;
_audit_creation_method           SHELXL-2012
_audit_update_record             'Tue Jan 22 16:37:12 CET 2013'
_cell_angle_alpha                90
_cell_angle_beta                 90.5118(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.36945(15)
_cell_length_b                   12.86281(10)
_cell_length_c                   17.41038(12)
_cell_measurement_reflns_used    26106
_cell_measurement_temperature    115(1)
_cell_measurement_theta_max      71.7133
_cell_measurement_theta_min      3.8163
_cell_volume                     3441.80(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_publication_material
'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      115(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   28.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 39

  2 omega  -19.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 78

  3 omega  -19.00   22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 41

  4 omega  -55.00   -2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  125.0000   30.0000 53

  5 omega -111.00  -74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 37

  6 omega  -39.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000    0.0000 27

  7 omega  -95.00  -69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 26

  8 omega  -55.00  -13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -120.0000 42

  9 omega  -65.00   11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   64.0000 -120.0000 76

 10 omega  -49.00   26.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000    0.0000 75

 11 omega  -24.00    2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -180.0000 26

 12 omega -103.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000 -180.0000 69

 13 omega  -41.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 29

 14 omega  -48.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 36

 15 omega  -37.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -30.0000 25

 16 omega -102.00  -53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000   30.0000 49

 17 omega  -63.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -180.0000 51

 18 omega  -44.00  -12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 32

 19 omega   74.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   76.0000  123.4463 34

 20 omega   25.00  125.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000  -30.0000 100

 21 omega   29.00  125.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000 -158.5639 96

 22 omega   30.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171 -125.0000   60.0000 82

 23 omega   25.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000   30.0000 40

 24 omega   27.00   53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   76.0000  123.4463 26

 25 omega   34.00  124.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   57.0000   90.0000 90

 26 omega   87.00  122.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   73.0000  158.3756 35

 27 omega   32.00   81.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   73.0000  158.3756 49

 28 omega   25.00  124.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000  -90.0000 99

 29 omega   58.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342 -111.0000   60.0000 58

 30 omega   88.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000    0.0000 27

 31 omega   38.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342 -111.0000  150.0000 61

 32 omega  113.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 64

 33 omega   89.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -60.0000 25

 34 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 26

 35 omega   84.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   71.0000   -4.6808 91

 36 omega   68.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342 -111.0000 -150.0000 48

 37 omega   88.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 87

 38 omega   88.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   60.0000 27

 39 omega  112.00  171.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 59

 40 omega   89.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 25

 41 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 26

 42 omega   84.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   71.0000   16.4956 26

 43 omega   84.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   37.0000  176.8402 26

 44 omega   41.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -50.0000 -120.0000 58

 45 omega  116.00  157.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 41

 46 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 26

 47 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 26

 48 omega   86.00  120.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 34

 49 omega   80.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 27

 50 omega   89.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -30.0000 85

 51 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

 52 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 26

 53 omega  117.00  173.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 56

 54 omega   80.00  173.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 93

 55 omega   80.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 31

 56 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 26

 57 omega   54.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -50.0000    0.0000 49

 58 omega   88.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  150.0000 26

 59 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

 60 omega   89.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   30.0000 26

 61 omega   88.00  165.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   90.0000 77

 62 omega   88.00  117.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 29

 63 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 26

 64 omega   86.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   41.0000 -158.2975 33

 65 omega   86.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 25

 66 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 26

 67 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 26

 68 omega   47.00  148.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -92.0000 -120.0000 101

 69 omega   41.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -50.0000  120.0000 63

 70 omega   85.00  112.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 27

 71 omega  111.00  171.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 60

 72 omega   86.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 25

 73 omega  140.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 34

 74 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

 75 omega   89.00  126.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   52.0000  -50.4171 37

 76 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   40.0000  113.9066 26

 77 omega  138.00  165.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   28.0000  -52.3204 27

 78 omega   79.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   28.0000  -52.3204 26

;
_diffrn_measurement_device       '\k-geometry 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_UB_11      -0.0022468000
_diffrn_orient_matrix_UB_12      -0.0155609000
_diffrn_orient_matrix_UB_13      0.0876998000
_diffrn_orient_matrix_UB_21      -0.0405704000
_diffrn_orient_matrix_UB_22      -0.1084502000
_diffrn_orient_matrix_UB_23      -0.0116551000
_diffrn_orient_matrix_UB_31      0.0916216000
_diffrn_orient_matrix_UB_32      -0.0483903000
_diffrn_orient_matrix_UB_33      -0.0021571000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52031
_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         71.858
_diffrn_reflns_theta_min         3.819
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    4.401
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.2060
_exptl_crystal_size_mid          0.1370
_exptl_crystal_size_min          0.1016
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0409P)^2^+4.4262P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6252
_reflns_number_total             6721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4004214_si_003_6.cif
_cod_data_source_block           co_mimo67
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335061
_audit_block_refno               1588
_audit_block_usercomment         'Mimo_482, irregular, blue'
_shelx_estimated_absorpt_t_min   0.464
_shelx_estimated_absorpt_t_max   0.663
_shelxl_version_number           2012-9
_shelx_res_checksum              2184
_cell_oxdiff_length_a            15.3713(3)
_cell_oxdiff_length_b            12.86251(19)
_cell_oxdiff_length_c            17.4087(2)
_cell_oxdiff_angle_alpha         90.0199(12)
_cell_oxdiff_angle_beta          90.5049(13)
_cell_oxdiff_angle_gamma         90.0057(14)
_cell_oxdiff_volume              3441.80(10)
_cell_oxdiff_measurement_reflns_used 26106
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1