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_4335066
_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_absolute_configuration unk
_chemical_formula_sum            'C25 H30 N4 O5'
_chemical_formula_weight         466.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           46
_space_group_name_Hall           'I 2 -2a'
_space_group_name_H-M_alt        'I m a 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      46
_symmetry_space_group_name_Hall  'I 2 -2a'
_symmetry_space_group_name_H-M   'I m a 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mimo35
_audit_creation_date
;
'Fri Jan 25 10:29:32 2013'
;
_audit_creation_method           SHELXL-2012
_audit_update_record             'Fri Jan 25 11:06:15 CET 2013'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7325(3)
_cell_length_b                   14.04059(14)
_cell_length_c                   7.83516(8)
_cell_measurement_reflns_used    14560
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      27.4350
_cell_measurement_theta_min      3.9950
_cell_volume                     2390.80(5)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_publication_material
'encif (Wadepohl, 2012); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega  -46.00   47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858  -79.0000   16.0000 93

  2 omega  -47.00   45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858  -77.0000  120.0000 92

  3 omega   14.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858   57.0000 -180.0000 26

  4 omega  -13.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858   77.0000   30.0000 99

  5 omega   -6.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858   57.0000  -60.0000 90

  6 omega   -7.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858   77.0000  150.0000 92

  7 omega  -56.00   15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858  -38.0000 -120.0000 71

  8 omega  -46.00  -13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   77.0000  120.0000 33

  9 omega  -46.00  -19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   77.0000   60.0000 27

 10 omega  -78.00  -45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327  -57.0000 -150.0000 33

 11 omega  -46.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   77.0000  150.0000 92

 12 omega  -46.00  -16.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   77.0000 -180.0000 30

 13 omega  -46.00  -20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   77.0000 -150.0000 26

 14 omega  -48.00   14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   80.0000  -45.0000 62

 15 omega  -48.00  -22.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   80.0000  -72.0000 26

 16 omega  -46.00  -17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   77.0000   30.0000 29

 17 omega  -48.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   80.0000 -117.0000 45

 18 omega  -15.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858   77.0000 -120.0000 101

 19 omega  -53.00   12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858  -57.0000   60.0000 65

 20 omega  -53.00   37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858  -57.0000  -90.0000 90

 21 omega  -15.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858   77.0000    0.0000 101

 22 omega  -53.00   37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3858  -57.0000  150.0000 90

 23 omega  -48.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327   80.0000 -117.0000 72

 24 omega  -85.00    5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9327  -57.0000   90.0000 90

;
_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      0.0321041000
_diffrn_orient_matrix_UB_12      -0.0038523000
_diffrn_orient_matrix_UB_13      0.0146829000
_diffrn_orient_matrix_UB_21      -0.0015023000
_diffrn_orient_matrix_UB_22      -0.0496343000
_diffrn_orient_matrix_UB_23      -0.0163601000
_diffrn_orient_matrix_UB_31      0.0056441000
_diffrn_orient_matrix_UB_32      0.0086088000
_diffrn_orient_matrix_UB_33      -0.0878290000
_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  0.0525
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            34290
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.865
_diffrn_reflns_theta_min         3.455
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 1158 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.3(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2794
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1105P)^2^+1.3122P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                2642
_reflns_number_total             2794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic4004214_si_004_4.cif
_cod_data_source_block           co_mimo35
_cod_original_cell_volume        2390.80(4)
_cod_database_code               4335066
_audit_block_refno               1336
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.990
_shelxl_version_number           2012-9
_shelx_res_checksum              20779
_cell_oxdiff_length_a            21.7370(6)
_cell_oxdiff_length_b            14.0393(3)
_cell_oxdiff_length_c            7.83426(15)
_cell_oxdiff_angle_alpha         89.9920(17)
_cell_oxdiff_angle_beta          90.0047(18)
_cell_oxdiff_angle_gamma         89.982(2)
_cell_oxdiff_volume              2390.80(10)
_cell_oxdiff_measurement_reflns_used 14560
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_theta     24.97
_reflns_odcompleteness_iscentric 1