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_4335058
_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            'C29 H38 Cl2 Cu N6 O14 S2'
_chemical_formula_weight         893.21
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mimo32a
_audit_creation_date
;
'Tue Sep 27 11:55:24 2011'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_cell_angle_alpha                65.620(4)
_cell_angle_beta                 79.171(4)
_cell_angle_gamma                65.285(4)
_cell_formula_units_Z            2.00000
_cell_length_a                   11.5947(5)
_cell_length_b                   13.4730(6)
_cell_length_c                   13.9099(5)
_cell_measurement_reflns_used    11551
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      72.0443
_cell_measurement_theta_min      3.4862
_cell_volume                     1797.57(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector_area_resol_mean 15.9241
_diffrn_measured_fraction_theta_full 0.984
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_diffrn_measurement_details
;
  1 omega  -21.00   61.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 82

  2 omega  -53.00  -15.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   30.0000 38

  3 omega  -44.00  -12.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -180.0000 32

  4 omega  -99.00  -34.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  -60.0000 65

  5 omega  -45.00  -12.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -120.0000 33

  6 omega  -43.00  -12.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  120.0000 31

  7 omega -105.00  -34.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  150.0000 71

  8 omega  -38.00  -12.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 26

  9 omega  -55.00   25.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   63.0000  -30.0000 80

 10 omega -101.00  -70.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 31

 11 omega -107.00  -71.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -60.0000 36

 12 omega  -63.00   18.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000  150.0000 81

 13 omega  -59.00   16.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   63.0000 -150.0000 75

 14 omega -106.00  -75.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -30.0000 31

 15 omega  -53.00  -14.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -60.0000 39

 16 omega  -40.00  -12.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -30.0000 28

 17 omega  -95.00  -57.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -120.0000 38

 18 omega   25.00  112.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -       55.1171 -125.0000   60.0000 87

 19 omega   26.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000 -180.0000 79

 20 omega   30.00  121.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -       55.1171   72.0000 -123.0000 91

 21 omega   26.00  125.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000  120.0000 99

 22 omega   25.00  125.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -       55.1171   77.0000   59.0000 100

 23 omega   27.00  122.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -       55.1171   76.0000  -25.0000 95

 24 omega   80.00  175.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 95

 25 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 25

 26 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 25

 27 omega   46.00  140.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000 -150.0000 94

 28 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 25

 29 omega   85.00  111.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 26

 30 omega   89.00  170.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  120.0000 81

 31 omega   85.00  118.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 33

 32 omega   42.00  111.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342 -111.0000   30.0000 69

 33 omega   89.00  115.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   60.0000 26

 34 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 25

 35 omega   88.00  175.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -30.0000 87

 36 omega   38.00  115.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342 -111.0000 -120.0000 77

 37 omega   80.00  175.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 95

 38 omega   80.00  110.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 30

 39 omega  114.00  177.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 63

 40 omega  128.00  167.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 39

 41 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 25

 42 omega  142.00  168.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

 43 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 25

 44 omega  124.00  163.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 39

 45 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 25

 46 omega  110.00  176.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 66

 47 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 25

 48 omega   88.00  114.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -90.0000 26

 49 omega   85.00  110.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  120.0000 25

 50 omega   90.00  115.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -180.0000 25

 51 omega   90.00  178.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 88

 52 omega   90.00  117.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 27

 53 omega   73.00  132.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -63.0000  -30.0000 59

 54 omega   89.00  115.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  150.0000 26

 55 omega   66.00  138.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000   60.0000 72

 56 omega   85.00  112.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 27

 57 omega   89.00  115.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -60.0000 26

 58 omega   85.00  110.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 25

 59 omega   89.00  115.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   57.0000    1.0000 26

 60 omega   85.00  110.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 25

 61 omega   85.00  110.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -180.0000 25

 62 omega   90.00  178.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000    0.0000 88

 63 omega  128.00  163.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 35

 64 omega   88.00  114.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342 -111.0000  150.0000 26

 65 omega   85.00  116.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 31

 66 omega   85.00  161.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -90.0000 76

 67 omega   80.00  105.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 25

 68 omega   86.00  121.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 35

 69 omega   96.00  121.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  120.0000 25

 70 omega   39.00   64.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342 -111.0000  150.0000 25

 71 omega   89.00  115.00   1.0000    3.2300
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   30.0000 26

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1027897000
_diffrn_orient_matrix_UB_12      0.0498346000
_diffrn_orient_matrix_UB_13      -0.0151832000
_diffrn_orient_matrix_UB_21      0.0049219000
_diffrn_orient_matrix_UB_22      0.0274010000
_diffrn_orient_matrix_UB_23      -0.1193902000
_diffrn_orient_matrix_UB_31      -0.1039758000
_diffrn_orient_matrix_UB_32      0.1232752000
_diffrn_orient_matrix_UB_33      -0.0174984000
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0880
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27485
_diffrn_reflns_theta_full        72.19
_diffrn_reflns_theta_max         72.0443
_diffrn_reflns_theta_min         3.4862
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    3.825
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
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    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.1476
_exptl_crystal_size_mid          0.1323
_exptl_crystal_size_min          0.0695
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         6992
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+1.6745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                6061
_reflns_number_total             6992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4004214_si_003_3.cif
_cod_data_source_block           co_mimo32a
_cod_original_cell_volume        1797.56(13)
_cod_database_code               4335058
_audit_block_refno               1331
_cell_oxdiff_length_a            11.5947(5)
_cell_oxdiff_length_b            13.4730(6)
_cell_oxdiff_length_c            13.9099(5)
_cell_oxdiff_angle_alpha         65.620(4)
_cell_oxdiff_angle_beta          79.171(4)
_cell_oxdiff_angle_gamma         65.285(4)
_cell_oxdiff_volume              1797.56(13)
_cell_oxdiff_measurement_reflns_used 11551
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         c25h30cl2cu1n4o12s2