Explosive Werner-type cobalt(iii) complexes
Deblitz, Raik; Hrib, Cristian G.; Blaurock, Steffen; Jones, Peter G.; Plenikowski, Georg; Edelmann, Frank T.; Inorg. Chem. Front. 1 (2014) 621–; doi:10.1039/C4QI00094C

data_4348258
_publ_section_title
;
 Explosive Werner-type cobalt(iii) complexes
;
_journal_issue                   8
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              621
_journal_paper_doi               10.1039/C4QI00094C
_journal_volume                  1
_journal_year                    2014
_chemical_formula_sum            'C H14 Co N11 O7'
_chemical_formula_weight         351.16
_space_group_IT_number           109
_space_group_name_Hall           'I 4bw -2'
_space_group_name_H-M_alt        'I 41 m d'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41 m d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8926(11)
_cell_length_b                   7.8926(11)
_cell_length_c                   19.125(4)
_cell_measurement_reflns_used    12862
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.79
_cell_volume                     1191.4(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6477
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.4303
_exptl_absorpt_correction_T_min  0.4187
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         855
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+0.4145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                849
_reflns_number_total             855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00094c2.cif
_cod_data_source_block           ip115
_cod_original_cell_volume        1191.3(3)
_cod_original_sg_symbol_H-M      I4(1)md
_cod_database_code               4348258
_exptl_absorpt_correction_t_ave  0.4254