Orientational disorder in Λ-cobalt(III) sepulchrate trinitrate
Schönleber, Andreas; van Smaalen, Sander; Larsen, Finn Krebs; Acta Crystallographica Section C 66 (2010) m107–m109; doi:10.1107/S0108270110005755

data_2017638
_publ_section_title
;
 Orientational disorder in \L-cobalt(III) sepulchrate trinitrate
;
_journal_coeditor_code           SU3043
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m107
_journal_page_last               m109
_journal_paper_doi               10.1107/S0108270110005755
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Co (C12 H30 N8)] (N O3)3'
_chemical_formula_moiety         'C12 H30 Co N8 3+ , 3N O3 -'
_chemical_formula_sum            'C12 H30 Co N11 O9'
_chemical_formula_weight         531.4
_chemical_name_common            Cobalt(sepulchrate)trinitrate
_chemical_name_systematic
;
[(1,3,6,8,10,13,16,19-octaazabicyclo[6.6.6]eicosane) cobalt(III) trinitrate
;
_space_group_IT_number           182
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   8.4945(5)
_cell_length_b                   8.4945(5)
_cell_length_c                   15.9195(13)
_cell_measurement_reflns_used    7040
_cell_measurement_temperature    295
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.5
_cell_volume                     994.80(12)
_computing_cell_refinement       'PEAKREF (Schreurs, 1999)'
_computing_data_collection       'MAR345DTB (Klein, 2003)'
_computing_data_reduction
;
EVAL15 (Schreurs <i>et al.</i>,  2010) and SADABS (Sheldrick,
2008)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material
'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>,  2006)'
_computing_structure_refinement
'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>,  2006)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      295
_diffrn_detector_area_resol_mean 0.15
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device       'one-circle diffractometer'
_diffrn_measurement_device_type  'MarIP mar345dtb'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0098
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49907
_diffrn_reflns_theta_full        34.62
_diffrn_reflns_theta_max         34.77
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.7734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.37
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.13(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.25
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    17
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.0029
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(\s^2^(F)+0.0004F^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0532
_reflns_number_gt                1322
_reflns_number_total             1404
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            su3043.cif
_cod_data_source_block           I
_cod_database_code               2017638
_cod_database_fobs_code          2017638