#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/99/2219961.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2219961
loop_
_publ_author_name
'Visser, Hendrik G.'
'Purcell, Walter'
_publ_section_title
;
 Hexaamminecobalt(III) hexacyanidomanganate(III)
;
_journal_coeditor_code           PK2122
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i76
_journal_paper_doi               10.1107/S1600536808032881
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Co (N H3)6] [Mn (C N)6]'
_chemical_formula_moiety         'Co H18 N6 3+, C6 Mn N6 3-'
_chemical_formula_sum            'C6 H18 Co Mn N12'
_chemical_formula_weight         372.19
_chemical_name_systematic
;
Hexaamminecobalt(III) hexacyanidomanganate(III)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                120.000
_cell_formula_units_Z            3
_cell_length_a                   10.963(5)
_cell_length_b                   10.963(5)
_cell_length_c                   10.779(5)
_cell_measurement_reflns_used    1532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.86
_cell_volume                     1121.9(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3602
_diffrn_reflns_theta_full        28.3
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    1.964
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.251
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.93
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.93
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0379P)²+3.8029P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                497
_reflns_number_total             628
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2122.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               2219961
_cod_database_fobs_code          2219961
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Co Co1 0 0 0 0.00732(17) Uani d S 1
Mn Mn1 0.3333 0.6667 0.1667 0.00607(17) Uani d S 1
N N1 -0.02748(15) 0.13048(15) -0.10659(13) 0.0107(3) Uani d . 1
H H1A 0.0238 0.2179 -0.0777 0.016 Uiso calc R 1
H H1B -0.1181 0.1061 -0.1065 0.016 Uiso calc R 1
H H1C -0.0006 0.1264 -0.1837 0.016 Uiso calc R 1
C C2 0.31385(18) 0.80238(18) 0.06080(16) 0.0119(3) Uani d . 1
N N2 0.30018(17) 0.87891(17) -0.00283(15) 0.0184(4) Uani d . 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 0.0076(2) 0.0076(2) 0.0067(3) 0.00381(10) 0 0
Mn1 0.0064(2) 0.0064(2) 0.0055(3) 0.00318(10) 0 0
N1 0.0117(7) 0.0099(7) 0.0111(7) 0.0058(6) 0.0007(5) 0.0010(5)
C2 0.0108(8) 0.0144(8) 0.0115(8) 0.0070(7) 0.0001(6) -0.0026(6)
N2 0.0200(8) 0.0248(9) 0.0159(7) 0.0152(7) 0.0014(6) 0.0013(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Co1 N1 11 2 180.00(7)
N1 Co1 N1 11 10 89.47(6)
N1 Co1 N1 2 10 90.53(6)
N1 Co1 N1 11 12 89.47(6)
N1 Co1 N1 2 12 90.53(6)
N1 Co1 N1 10 12 89.47(6)
N1 Co1 N1 11 . 90.53(6)
N1 Co1 N1 2 . 89.47(6)
N1 Co1 N1 10 . 180.00(10)
N1 Co1 N1 12 . 90.53(6)
N1 Co1 N1 11 3 90.53(6)
N1 Co1 N1 2 3 89.47(6)
N1 Co1 N1 10 3 90.53(6)
N1 Co1 N1 12 3 180.00(10)
N1 Co1 N1 . 3 89.47(6)
C2 Mn1 C2 13_565 . 180
C2 Mn1 C2 13_565 2_665 90.20(7)
C2 Mn1 C2 . 2_665 89.80(7)
C2 Mn1 C2 13_565 3_565 90.20(7)
C2 Mn1 C2 . 3_565 89.80(7)
C2 Mn1 C2 2_665 3_565 89.80(7)
C2 Mn1 C2 13_565 14_455 89.80(7)
C2 Mn1 C2 . 14_455 90.20(7)
C2 Mn1 C2 2_665 14_455 180
C2 Mn1 C2 3_565 14_455 90.20(7)
C2 Mn1 C2 13_565 15 89.80(7)
C2 Mn1 C2 . 15 90.20(7)
C2 Mn1 C2 2_665 15 90.20(7)
C2 Mn1 C2 3_565 15 180.00(7)
C2 Mn1 C2 14_455 15 89.80(7)
Co1 N1 H1A . . 109.5
Co1 N1 H1B . . 109.5
H1A N1 H1B . . 109.5
Co1 N1 H1C . . 109.5
H1A N1 H1C . . 109.5
H1B N1 H1C . . 109.5
N2 C2 Mn1 . . 178.31(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 N1 11 1.9718(16)
Co1 N1 2 1.9718(16)
Co1 N1 10 1.9718(15)
Co1 N1 12 1.9718(15)
Co1 N1 . 1.9718(15)
Co1 N1 3 1.9718(15)
Mn1 C2 13_565 1.9696(19)
Mn1 C2 . 1.9696(19)
Mn1 C2 2_665 1.9696(19)
Mn1 C2 3_565 1.9696(19)
Mn1 C2 14_455 1.9696(19)
Mn1 C2 15 1.9696(19)
N1 H1A . 0.89
N1 H1B . 0.89
N1 H1C . 0.89
C2 N2 . 1.150(2)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A N2 2_665 0.89 2.09 2.979(2) 172.9
