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_4335059
_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            'C25 H32.3 Cl2 Cu N4 O16.15'
_chemical_formula_weight         781.69
_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   mixed
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_audit_block_code                co_mimo40
_audit_creation_date
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'Thu Jan 24 17:18:06 2013'
;
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_audit_update_record             'Thu Jan 24 17:22:25 CET 2013'
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'
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_diffrn_measurement_details
;
  1 omega  -40.00   18.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -19.0000  150.0000 58

  2 omega  -44.00   58.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -79.0000   55.0000 102

  3 omega   23.00   59.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -19.0000  150.0000 36

  4 omega   -4.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   77.0000  -90.0000 101

  5 omega    5.00   78.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   57.0000 -150.0000 73

  6 omega    2.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   38.0000   60.0000 88

  7 omega   -4.00   96.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   77.0000   90.0000 100

  8 omega  -40.00   58.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -80.0000  150.0000 98

  9 omega  -36.00   56.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -77.0000  -30.0000 92

 10 omega  -23.00    3.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224  -77.0000  -90.0000 26

 11 omega  -97.00  -71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224  -77.0000  -90.0000 26

 12 omega  -59.00   22.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224   80.0000 -116.0000 81

 13 omega  -42.00   48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -57.0000  -90.0000 90

 14 omega   -4.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   77.0000   30.0000 101

 15 omega  -42.00   48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -57.0000  120.0000 90

 16 omega    5.00   95.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   57.0000  -90.0000 90

 17 omega   -4.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   77.0000  150.0000 101

 18 omega    5.00   95.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   57.0000  120.0000 90

 19 omega    1.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974   38.0000   30.0000 98

 20 omega  -57.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224   77.0000  -30.0000 100

 21 omega  -59.00   24.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224   80.0000 -116.0000 83

 22 omega  -59.00   24.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224   80.0000  170.0000 83

 23 omega  -47.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974    0.0000    0.0000 146

 24 omega  -44.00   58.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -79.0000   55.0000 102

 25 omega  -44.00   56.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -77.0000 -150.0000 100

 26 omega  -44.00   56.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -77.0000   90.0000 100

 27 omega  -44.00   58.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -80.0000  150.0000 102

 28 omega  -44.00   58.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -80.0000   30.0000 102

 29 omega  -44.00   56.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974  -77.0000  -60.0000 100

 30 omega  -97.00    3.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224  -77.0000 -150.0000 100

 31 omega  -57.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224   77.0000   90.0000 100

 32 omega  -57.00   43.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.0224   77.0000   30.0000 100

 33 omega  -47.00   -8.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3974    0.0000  120.0000 39

;
_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      -0.0047118000
_diffrn_orient_matrix_UB_12      0.0455578000
_diffrn_orient_matrix_UB_13      -0.0225313000
_diffrn_orient_matrix_UB_21      -0.0518179000
_diffrn_orient_matrix_UB_22      0.0010341000
_diffrn_orient_matrix_UB_23      0.0042082000
_diffrn_orient_matrix_UB_31      0.0084011000
_diffrn_orient_matrix_UB_32      0.0320759000
_diffrn_orient_matrix_UB_33      0.0318407000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            164921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         27.187
_diffrn_reflns_theta_min         3.394
_diffrn_source                   'microfocus X-Ray tube'
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       needle
_exptl_crystal_F_000             1610
_exptl_crystal_size_max          0.2878
_exptl_crystal_size_mid          0.0737
_exptl_crystal_size_min          0.0614
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         6895
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0319P)^2^+11.0949P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6126
_reflns_number_total             6895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4004214_si_003_4.cif
_cod_data_source_block           co_mimo40
_cod_original_cell_volume        3105.69(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C25 H32.30 Cl2 Cu N4 O16.15'
_cod_database_code               4335059
_audit_block_refno               1379
_audit_block_usercomment         Mimo_408
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2012-9
_shelx_res_checksum              98000
_cell_oxdiff_length_a            13.4960(3)
_cell_oxdiff_length_b            12.7282(2)
_cell_oxdiff_length_c            18.1308(3)
_cell_oxdiff_angle_alpha         89.9770(13)
_cell_oxdiff_angle_beta          94.3156(15)
_cell_oxdiff_angle_gamma         90.0256(14)
_cell_oxdiff_volume              3105.69(9)
_cell_oxdiff_measurement_reflns_used 23549
_reflns_odcompleteness_completeness 72.97
_reflns_odcompleteness_theta     30.44
_reflns_odcompleteness_iscentric 1