#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/57/4505784.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4505784
loop_
_publ_author_name
'Saha, Manas K.'
'Ramanujam, Rathnakumar'
'Bernal, Ivan'
'Fronczek, Frank R.'
_publ_section_title
;
 The Phenomenon of Conglomerate Crystallization. Part 57. Control of the
 Crystallization Behavior by the Choice of the Counter Ion. Part 9. The
 Stereochemistry and Crystallization Architecture of [(3,2,3-tet)Co(N3)2]X
 (X = Cl(I), Br(II), I(III), NO3(IV), and PF6(V))
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              205
_journal_paper_doi               10.1021/cg020003i
_journal_volume                  2
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C8 H22 Co1 I1 N10'
_chemical_formula_structural     'C8 H22 CO I N10'
_chemical_formula_sum            'C8 H22 Co I N10'
_chemical_formula_weight         444.19
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2001-09-18T10:17:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.6949(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0255(2)
_cell_length_b                   10.3728(2)
_cell_length_c                   15.0556(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1563.94(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.074
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17863
_diffrn_reflns_theta_full        40.18
_diffrn_reflns_theta_max         40.18
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    3.08
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.979
_refine_diff_density_min         -1.553
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         9768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0296P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                6407
_reflns_number_total             9768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg020003i_s3.cif
_cod_data_source_block           struct
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C8 H22 Co1 I1 N10'
_cod_database_code               4505784
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.01930(19) 0.16237(19) 0.37583(14) 0.0150(3) Uani 1 1 d . . .
C2 C -0.02068(19) 0.2023(2) 0.46804(14) 0.0160(3) Uani 1 1 d . . .
C3 C 0.08006(19) 0.1631(2) 0.54147(13) 0.0156(3) Uani 1 1 d . . .
C4 C 0.2999(2) 0.1979(2) 0.61224(13) 0.0161(3) Uani 1 1 d . . .
C5 C 0.4327(2) 0.2610(2) 0.59753(13) 0.0163(3) Uani 1 1 d . . .
C6 C 0.59286(18) 0.29610(19) 0.48176(13) 0.0147(3) Uani 1 1 d . . .
C7 C 0.63594(19) 0.2591(2) 0.39004(14) 0.0161(3) Uani 1 1 d . . .
C8 C 0.53852(19) 0.30414(19) 0.31655(13) 0.0146(3) Uani 1 1 d . . .
Co Co 0.30711(2) 0.23018(2) 0.426039(16) 0.00906(5) Uani 1 1 d . . .
I I 0.088980(13) 0.492898(12) 0.684361(9) 0.01862(4) Uani 1 1 d . . .
N1 N 0.14089(15) 0.23250(16) 0.34902(11) 0.0123(3) Uani 1 1 d . . .
N2 N 0.20770(15) 0.23493(15) 0.53712(11) 0.0124(3) Uani 1 1 d . . .
N3 N 0.47054(16) 0.22539(16) 0.50633(10) 0.0119(3) Uani 1 1 d . . .
N4 N 0.40936(15) 0.23206(16) 0.31709(11) 0.0122(3) Uani 1 1 d . . .
N5 N 0.30730(16) 0.41738(14) 0.43411(11) 0.0135(3) Uani 1 1 d . . .
N6 N 0.30250(16) 0.49025(14) 0.37140(11) 0.0132(3) Uani 1 1 d . . .
N7 N 0.30128(19) 0.56733(17) 0.31541(12) 0.0215(4) Uani 1 1 d . . .
N8 N 0.31724(16) 0.03992(15) 0.43453(11) 0.0145(3) Uani 1 1 d . . .
N9 N 0.27264(17) -0.03805(16) 0.38277(11) 0.0146(3) Uani 1 1 d . . .
N10 N 0.2316(2) -0.12060(18) 0.33805(14) 0.0296(5) Uani 1 1 d . . .
H1 H 0.159(2) 0.201(2) 0.2944(17) 0.013(6) Uiso 1 1 d . . .
H2 H 0.123(3) 0.310(3) 0.3392(18) 0.023(7) Uiso 1 1 d . . .
H3 H 0.041(2) 0.065(2) 0.3731(16) 0.017(6) Uiso 1 1 d . . .
H4 H -0.050(2) 0.181(3) 0.3316(17) 0.022(7) Uiso 1 1 d . . .
H5 H -0.036(2) 0.288(2) 0.4700(16) 0.014(6) Uiso 1 1 d . . .
H6 H -0.109(3) 0.161(3) 0.4764(18) 0.030(7) Uiso 1 1 d . . .
H7 H 0.046(2) 0.185(2) 0.5997(16) 0.015(6) Uiso 1 1 d . . .
H8 H 0.097(2) 0.071(2) 0.5357(17) 0.021(6) Uiso 1 1 d . . .
H9 H 0.191(2) 0.314(2) 0.5450(15) 0.011(6) Uiso 1 1 d . . .
H10 H 0.265(3) 0.226(2) 0.6669(17) 0.020(6) Uiso 1 1 d . . .
H11 H 0.307(2) 0.112(2) 0.6137(15) 0.012(6) Uiso 1 1 d . . .
H12 H 0.424(2) 0.358(2) 0.5962(16) 0.016(6) Uiso 1 1 d . . .
H13 H 0.496(3) 0.230(2) 0.6393(17) 0.018(6) Uiso 1 1 d . . .
H14 H 0.484(2) 0.158(3) 0.5085(17) 0.023(8) Uiso 1 1 d . . .
H15 H 0.568(2) 0.389(2) 0.4851(14) 0.007(5) Uiso 1 1 d . . .
H16 H 0.664(3) 0.273(2) 0.5314(18) 0.023(7) Uiso 1 1 d . . .
H17 H 0.651(2) 0.164(2) 0.3818(17) 0.023(7) Uiso 1 1 d . . .
H18 H 0.720(2) 0.305(2) 0.3817(15) 0.014(6) Uiso 1 1 d . . .
H19 H 0.522(2) 0.397(2) 0.3258(14) 0.006(5) Uiso 1 1 d . . .
H20 H 0.580(2) 0.286(2) 0.2595(16) 0.015(6) Uiso 1 1 d . . .
H21 H 0.423(3) 0.149(3) 0.296(2) 0.039(8) Uiso 1 1 d . . .
H22 H 0.355(3) 0.266(3) 0.271(2) 0.031(8) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_number_in_cell
C 32
H 88
Co 4
I 4
N 40
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 C1 C2 111.59(16) . .
N1 C1 H3 107.0(13) . .
C2 C1 H3 111.5(13) . .
N1 C1 H4 106.6(15) . .
C2 C1 H4 111.4(15) . .
H3 C1 H4 109(2) . .
C3 C2 C1 113.39(16) . .
C3 C2 H5 110.6(17) . .
C1 C2 H5 110.6(15) . .
C3 C2 H6 110.8(16) . .
C1 C2 H6 105.7(16) . .
H5 C2 H6 105(2) . .
N2 C3 C2 112.25(16) . .
N2 C3 H7 105.0(14) . .
C2 C3 H7 109.7(14) . .
N2 C3 H8 109.3(14) . .
C2 C3 H8 108.2(15) . .
H7 C3 H8 112(2) . .
N2 C4 C5 107.43(15) . .
N2 C4 H10 109.7(15) . .
C5 C4 H10 111.1(15) . .
N2 C4 H11 108.8(15) . .
C5 C4 H11 111.6(15) . .
H10 C4 H11 108(2) . .
N3 C5 C4 107.02(16) . .
N3 C5 H12 104.8(14) . .
C4 C5 H12 110.9(13) . .
N3 C5 H13 110.1(15) . .
C4 C5 H13 109.2(15) . .
H12 C5 H13 115(2) . .
N3 C6 C7 112.00(16) . .
N3 C6 H15 104.5(12) . .
C7 C6 H15 112.0(13) . .
N3 C6 H16 105.0(14) . .
C7 C6 H16 112.4(14) . .
H15 C6 H16 110.5(18) . .
C8 C7 C6 112.70(16) . .
C8 C7 H17 107.9(15) . .
C6 C7 H17 114.4(14) . .
C8 C7 H18 106.6(14) . .
C6 C7 H18 106.1(14) . .
H17 C7 H18 108.9(19) . .
N4 C8 C7 111.74(16) . .
N4 C8 H19 109.8(12) . .
C7 C8 H19 107.6(13) . .
N4 C8 H20 108.1(14) . .
C7 C8 H20 106.8(14) . .
H19 C8 H20 112.9(18) . .
N5 Co N4 92.46(7) . .
N5 Co N8 172.25(7) . .
N4 Co N8 92.09(7) . .
N5 Co N1 91.30(7) . .
N4 Co N1 88.22(7) . .
N8 Co N1 95.10(7) . .
N5 Co N2 85.51(7) . .
N4 Co N2 177.70(7) . .
N8 Co N2 89.81(7) . .
N1 Co N2 92.91(7) . .
N5 Co N3 89.34(7) . .
N4 Co N3 93.44(7) . .
N8 Co N3 84.13(7) . .
N1 Co N3 178.19(7) . .
N2 Co N3 85.45(6) . .
C1 N1 Co 120.69(13) . .
C1 N1 H1 105.7(14) . .
Co N1 H1 108.9(15) . .
C1 N1 H2 110.1(18) . .
Co N1 H2 106.5(18) . .
H1 N1 H2 104(2) . .
C4 N2 C3 110.20(15) . .
C4 N2 Co 108.50(11) . .
C3 N2 Co 119.47(12) . .
C4 N2 H9 105.3(16) . .
C3 N2 H9 107.9(15) . .
Co N2 H9 104.5(15) . .
C5 N3 C6 110.80(15) . .
C5 N3 Co 108.43(12) . .
C6 N3 Co 120.03(12) . .
C5 N3 H14 105(2) . .
C6 N3 H14 110(2) . .
Co N3 H14 102(2) . .
C8 N4 Co 119.53(12) . .
C8 N4 H21 108.5(17) . .
Co N4 H21 111.4(18) . .
C8 N4 H22 106.3(17) . .
Co N4 H22 108.5(17) . .
H21 N4 H22 101(2) . .
N6 N5 Co 125.13(13) . .
N7 N6 N5 175.0(2) . .
N9 N8 Co 128.01(14) . .
N10 N9 N8 174.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.491(2) .
C1 C2 1.521(3) .
C1 H3 1.03(2) .
C1 H4 0.96(3) .
C2 C3 1.518(3) .
C2 H5 0.91(2) .
C2 H6 1.00(3) .
C3 N2 1.485(2) .
C3 H7 0.98(2) .
C3 H8 0.98(3) .
C4 N2 1.478(3) .
C4 C5 1.509(3) .
C4 H10 0.96(3) .
C4 H11 0.90(2) .
C5 N3 1.488(2) .
C5 H12 1.01(2) .
C5 H13 0.93(3) .
C6 N3 1.490(2) .
C6 C7 1.516(3) .
C6 H15 1.00(2) .
C6 H16 1.04(3) .
C7 C8 1.515(3) .
C7 H17 1.00(3) .
C7 H18 0.98(2) .
C8 N4 1.496(2) .
C8 H19 0.98(2) .
C8 H20 0.99(2) .
Co N5 1.9456(15) .
Co N4 1.9748(15) .
Co N8 1.9799(16) .
Co N1 1.9851(16) .
Co N2 1.9873(15) .
Co N3 1.9904(16) .
N1 H1 0.91(2) .
N1 H2 0.84(3) .
N2 H9 0.85(2) .
N3 H14 0.72(3) .
N4 H21 0.93(3) .
N4 H22 0.93(3) .
N5 N6 1.209(2) .
N6 N7 1.161(2) .
N8 N9 1.195(2) .
N9 N10 1.153(2) .
