The azide-bridged mixed-valent cobalt(II,III) compound [(CH~3~)~3~NH]~2~[Co^II^Co~2~^III^(N~3~)~10~]
Liu, Yan-Ju; Li, Yu-Xian; Xu, Min; Wang, Xia; Acta Crystallographica Section E 67 (2011) m27–; doi:10.1107/S1600536810049421

data_2228902
_publ_section_title
;
 The azide-bridged mixed-valent cobalt(II,III) compound
 [(CH~3~)~3~NH]~2~[Co^II^Co~2~^III^(N~3~)~10~]
;
_journal_coeditor_code           WM2430
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m27
_journal_paper_doi               10.1107/S1600536810049421
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C3 H10 N)2 [Co3 (N3)10]'
_chemical_formula_moiety         'Co3 N30, 2(C3 H10 N)'
_chemical_formula_sum            'C6 H20 Co3 N32'
_chemical_formula_weight         717.33
_chemical_name_systematic
;
poly[bis(trimethylammonium) [hexa-\m~1,1~-azido-tetraazidotricobaltate(II,III)]]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 115.524(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7200(6)
_cell_length_b                   11.3812(4)
_cell_length_c                   12.1628(4)
_cell_measurement_reflns_used    14377
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.395
_cell_volume                     2713.21(16)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       'dtprofit.ref scans'
_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  0.1028
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22049
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>REQAB</i>; Jacobson, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.346
_refine_ls_extinction_coef       0.00084(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2389
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                1481
_reflns_number_total             2389
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2430.cif
_cod_data_source_block           I
_cod_original_cell_volume        2713.21(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2228902
_cod_database_fobs_code          2228902