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_4302662
_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            'C32 H44 Cl2 N6 O9 Zn'
_chemical_formula_weight         793.00
_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_ch24
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.402(14)
_cell_angle_beta                 80.665(14)
_cell_angle_gamma                85.691(12)
_cell_formula_units_Z            2
_cell_length_a                   10.273(5)
_cell_length_b                   11.535(5)
_cell_length_c                   15.223(7)
_cell_measurement_reflns_used    8138
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.08
_cell_measurement_theta_min      2.61
_cell_volume                     1735.7(14)
_computing_cell_refinement
;

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

 of the unit cell constants 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, 1980-2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43613
_diffrn_reflns_theta_full        32.20
_diffrn_reflns_theta_max         32.20
_diffrn_reflns_theta_min         1.81
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6700
_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            colourless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.085
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         11411
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+1.6473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                9680
_reflns_number_total             11411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900571v_si_001_05.cif
_cod_data_source_block           co_ch24
_cod_database_code               4302662
_audit_block_refno               855