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_4335051
_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            'C20 H19 Br2 N3 O5'
_chemical_formula_weight         541.20
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mimo36
_audit_creation_date
;
'Fri Oct 21 17:24:30 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                99.7871(17)
_cell_angle_beta                 99.9915(17)
_cell_angle_gamma                104.9935(17)
_cell_formula_units_Z            4.00000
_cell_length_a                   13.1630(3)
_cell_length_b                   13.1895(3)
_cell_length_c                   13.4888(3)
_cell_measurement_reflns_used    24167
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      27.4241
_cell_measurement_theta_min      3.1956
_cell_volume                     2170.23(9)
_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    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector_area_resol_mean 15.9241
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -2.00   76.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817   57.0000  -60.0000 78

  2 omega  -44.00   48.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -77.0000    0.0000 92

  3 omega   -3.00   87.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817   57.0000   30.0000 90

  4 omega   34.00   90.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817   19.0000  -90.0000 56

  5 omega   18.00   47.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -77.0000   30.0000 29

  6 omega  -50.00    2.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -57.0000 -120.0000 52

  7 omega   -9.00   89.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817   77.0000  120.0000 98

  8 omega  -46.00   47.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -77.0000  120.0000 93

  9 omega  -49.00  -12.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000 -120.0000 37

 10 omega  -62.00   -2.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286  -77.0000 -180.0000 60

 11 omega  -49.00   28.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000  -90.0000 77

 12 omega  -48.00  -22.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000 -180.0000 26

 13 omega    5.00   41.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000  150.0000 36

 14 omega  -49.00  -17.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000  150.0000 32

 15 omega  -49.00  -23.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000 -150.0000 26

 16 omega  -51.00  -25.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   80.0000   43.0000 26

 17 omega  -50.00   40.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -57.0000  120.0000 90

 18 omega  -12.00   89.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817   77.0000   30.0000 101

 19 omega   -3.00   87.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817   57.0000 -180.0000 90

 20 omega  -50.00   40.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -57.0000   30.0000 90

 21 omega  -52.00   48.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -77.0000    0.0000 100

 22 omega  -50.00   40.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -57.0000   60.0000 90

 23 omega  -54.00   44.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -38.0000  150.0000 98

 24 omega  -55.00   62.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -       18.3817  -19.0000 -180.0000 117

 25 omega  -88.00    2.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286  -57.0000  150.0000 90

 26 omega  -49.00   51.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000 -150.0000 100

 27 omega  -49.00   51.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000  -90.0000 100

 28 omega  -51.00   24.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   80.0000   43.0000 75

 29 omega  -89.00   11.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286  -77.0000   30.0000 100

 30 omega  -49.00   18.00   1.0000    8.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.9286   77.0000 -120.0000 67

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0127483000
_diffrn_orient_matrix_UB_12      -0.0087155000
_diffrn_orient_matrix_UB_13      0.0474380000
_diffrn_orient_matrix_UB_21      0.0506865000
_diffrn_orient_matrix_UB_22      0.0368358000
_diffrn_orient_matrix_UB_23      0.0273260000
_diffrn_orient_matrix_UB_31      -0.0234885000
_diffrn_orient_matrix_UB_32      0.0428171000
_diffrn_orient_matrix_UB_33      0.0026719000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.1437
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            94078
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.4241
_diffrn_reflns_theta_min         3.1956
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    3.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68784
_exptl_absorpt_correction_type   multi-scan
_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)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.8754
_exptl_crystal_size_mid          0.3302
_exptl_crystal_size_min          0.1828
_refine_diff_density_max         2.038
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         9927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+3.7238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                8226
_reflns_number_total             9927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4004214_si_002_2.cif
_cod_data_source_block           co_mimo36
_cod_original_cell_volume        2170.22(7)
_cod_database_code               4335051
_audit_block_refno               1340
_cell_oxdiff_length_a            13.1630(3)
_cell_oxdiff_length_b            13.1895(3)
_cell_oxdiff_length_c            13.4888(3)
_cell_oxdiff_angle_alpha         99.7871(17)
_cell_oxdiff_angle_beta          99.9915(17)
_cell_oxdiff_angle_gamma         104.9935(17)
_cell_oxdiff_volume              2170.22(7)
_cell_oxdiff_measurement_reflns_used 24167
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         C20H19Br2N3O5