Novel Bispidine Ligands and Their First-Row Transition Metal Complexes: Trigonal Bipyramidal and Trigonal Prismatic Geometries
Peter Comba; Christina Haaf; Hubert Wadepohl; Inorganic Chemistry 48 (2009) 6604–6614; doi:10.1021/ic900571v

data_4302667
_publ_section_title
;
Novel Bispidine Ligands and Their First-Row Transition Metal Complexes:
Trigonal Bipyramidal and Trigonal Prismatic Geometries
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6604
_journal_page_last               6614
_journal_paper_doi               10.1021/ic900571v
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C33 H41.53 Cl2 N5 Ni O9.27'
_chemical_formula_weight         786.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                co_ch13
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.471(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.739(7)
_cell_length_b                   19.904(11)
_cell_length_c                   16.368(9)
_cell_measurement_reflns_used    8148
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.85
_cell_measurement_theta_min      2.30
_cell_volume                     3388(3)
_computing_cell_refinement
;

SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors

 from Monte Carlo simulations.

;
_computing_data_collection       'SMART (Bruker AXS, 1997-2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2008)'
_computing_molecular_graphics    'PLATON (Spek, 1980-2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'PLATON/FLIPPER (Spek, 2007-2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'CCD area detector (Bruker AXS Smart 1000)'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            73062
_diffrn_reflns_theta_full        32.11
_diffrn_reflns_theta_max         32.11
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

multi-scan from symmetry-related measurements (Blessing 1995)

SADABS (Sheldrick & Bruker AXS, 2004-2008)

;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1643
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         11145
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.332
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0308P)^2^+6.4967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                7803
_reflns_number_total             11145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900571v_si_001_10.cif
_cod_data_source_block           co_ch13
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302667
_audit_block_refno               793