#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:02:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179464 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/61/4336165.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_4336165
loop_
_publ_author_name
'Lai-Chin Wu'
'Tsu-Chien Weng'
'I-Jui Hsu'
'Yi-Hung Liu'
'Gene-Hsiang Lee'
'Jyh-Fu, Lee'
'Yu Wang'
_publ_section_title
;
 Chemical Bond Characterization of a Mixed-Valence Tri-Cobalt Complex,
 Co3(μ-admtrz)4(μ-OH)2(CN)6.2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11023
_journal_page_last               11033
_journal_paper_doi               10.1021/ic401147b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C22 H42 Co3 N22 O6'
_chemical_formula_weight         887.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.0260(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.82740(10)
_cell_length_b                   9.82110(8)
_cell_length_c                   17.73730(2)
_cell_measurement_reflns_used    583
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      5
_cell_volume                     1837.60(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford CCD diffractometer'
_diffrn_measurement_method       'Omega scan+phi scan'
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            153502
_diffrn_reflns_theta_full        48.67
_diffrn_reflns_theta_max         48.67
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.8515
_exptl_absorpt_correction_T_min  0.7224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
A combination of a face-indexed absorption and a multi-scan 
correction (in SADABS) was applied.
The crystal faces were indexed, and distances measured using the CrystAlis
software.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         18076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0349P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                12653
_reflns_number_total             18076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401147b_si_002.cif
_cod_data_source_block           ic13189
_cod_database_code               4336165
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Co1 Co -0.201466(7) 0.881991(8) 0.847947(4) 0.00989(1) Uani 1 1 d . . .
Co2 Co 0.0000 1.0000 1.0000 0.00878(2) Uani 1 2 d S . .
C1 C -0.36266(6) 0.84801(6) 0.86303(4) 0.01502(9) Uani 1 1 d . . .
C2 C -0.26379(6) 0.91137(7) 0.74129(3) 0.01565(9) Uani 1 1 d . . .
C3 C -0.19155(6) 0.69525(7) 0.83299(4) 0.01624(10) Uani 1 1 d . . .
C4 C 0.03980(5) 0.85491(6) 0.78628(3) 0.01259(8) Uani 1 1 d . . .
C5 C -0.00625(7) 0.77955(8) 0.71317(4) 0.02004(12) Uani 1 1 d . . .
C6 C 0.17580(5) 0.95080(6) 0.88215(3) 0.01216(8) Uani 1 1 d . . .
C7 C 0.29770(6) 0.99804(8) 0.93113(4) 0.02025(12) Uani 1 1 d . . .
C8 C 0.17786(5) 0.74480(6) 1.05219(3) 0.01283(8) Uani 1 1 d . . .
C9 C 0.11594(7) 0.64604(7) 0.99245(5) 0.02107(12) Uani 1 1 d . . .
C10 C 0.32027(5) 0.83630(6) 1.14660(3) 0.01240(8) Uani 1 1 d . . .
C11 C 0.44139(6) 0.85293(7) 1.20435(4) 0.01749(10) Uani 1 1 d . . .
N1 N -0.46178(6) 0.82572(7) 0.87450(4) 0.02369(12) Uani 1 1 d . . .
N2 N -0.29681(6) 0.93093(8) 0.67540(3) 0.02402(12) Uani 1 1 d . . .
N3 N -0.18658(7) 0.57823(7) 0.82738(4) 0.02556(12) Uani 1 1 d . . .
N4 N -0.02339(4) 0.90323(5) 0.83622(3) 0.01123(7) Uani 1 1 d . . .
N5 N 0.06290(4) 0.96173(5) 0.89699(3) 0.01110(7) Uani 1 1 d . . .
N6 N 0.16451(5) 0.88416(5) 0.81378(3) 0.01219(7) Uani 1 1 d . . .
N7 N 0.26015(5) 0.84711(6) 0.77607(3) 0.01576(8) Uani 1 1 d . . .
N8 N 0.13538(5) 0.86467(5) 1.06697(3) 0.01138(7) Uani 1 1 d . . .
N9 N 0.22451(4) 0.92228(5) 1.12685(3) 0.01097(7) Uani 1 1 d . . .
N10 N 0.29289(5) 0.72413(5) 1.10096(3) 0.01310(7) Uani 1 1 d . . .
N11 N 0.37219(6) 0.60972(6) 1.10561(4) 0.01840(9) Uani 1 1 d . . .
O1 O -0.12876(4) 0.85935(4) 0.95545(2) 0.01177(6) Uani 1 1 d . . .
O2 O 0.73054(6) 0.66296(6) 1.02308(4) 0.02659(11) Uani 1 1 d . . .
O3A O 0.3856(14) 0.6394(7) 0.9401(4) 0.0378(17) Uani 0.40(2) 1 d P A 1
O3B O 0.4373(7) 0.6210(3) 0.94774(11) 0.0305(7) Uani 0.60(2) 1 d P A 2
H1 H 0.2681(10) 0.9151(11) 0.7459(6) 0.021(2) Uiso 1 1 d . . .
H2 H 0.3297(11) 0.8358(11) 0.8107(6) 0.024(3) Uiso 1 1 d . . .
H3 H 0.3975(13) 0.5978(13) 1.0646(8) 0.038(3) Uiso 1 1 d . . .
H4 H 0.3293(11) 0.5376(13) 1.1130(7) 0.029(3) Uiso 1 1 d . . .
H1A H -0.1581(11) 0.8092(13) 0.9752(7) 0.027(3) Uiso 1 1 d . . .
H2A H 0.6471(18) 0.6626(18) 0.9964(10) 0.071(5) Uiso 1 1 d . . .
H2B H 0.7230(15) 0.6361(15) 1.0706(10) 0.052(4) Uiso 1 1 d . . .
H3A H 0.4448(13) 0.6839(15) 0.9211(8) 0.039(3) Uiso 1 1 d . . .
H3B H 0.3915(16) 0.5732(18) 0.9181(9) 0.055(5) Uiso 1 1 d . . .
H5A H 0.0554(13) 0.7132(13) 0.7087(8) 0.039(3) Uiso 1 1 d . . .
H5B H -0.0111(15) 0.8429(17) 0.6749(9) 0.055(4) Uiso 1 1 d . . .
H5C H -0.0863(12) 0.7443(12) 0.7120(7) 0.032(3) Uiso 1 1 d . . .
H7A H 0.2827(11) 1.0294(12) 0.9781(7) 0.028(3) Uiso 1 1 d . . .
H7B H 0.3561(13) 0.9287(14) 0.9376(7) 0.038(3) Uiso 1 1 d . . .
H7C H 0.3277(13) 1.0714(14) 0.9065(8) 0.042(3) Uiso 1 1 d . . .
H9A H 0.1100(14) 0.5631(16) 1.0154(8) 0.047(4) Uiso 1 1 d . . .
H9B H 0.0315(11) 0.6760(12) 0.9693(7) 0.027(3) Uiso 1 1 d . . .
H9C H 0.1686(12) 0.6369(12) 0.9537(7) 0.030(3) Uiso 1 1 d . . .
H11A H 0.4951(14) 0.9081(15) 1.1840(8) 0.047(4) Uiso 1 1 d . . .
H11B H 0.4829(12) 0.7649(13) 1.2163(7) 0.036(3) Uiso 1 1 d . . .
H11C H 0.4275(12) 0.8957(12) 1.2460(8) 0.034(3) Uiso 1 1 d . . .
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 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Co1 C3 85.96(3) . .
C1 Co1 C2 92.11(3) . .
C3 Co1 C2 91.54(3) . .
C1 Co1 O1 91.41(2) . .
C3 Co1 O1 90.20(2) . .
C2 Co1 O1 176.18(2) . .
C1 Co1 N4 175.05(2) . .
C3 Co1 N4 90.00(2) . .
C2 Co1 N4 90.87(2) . .
O1 Co1 N4 85.732(19) . .
C1 Co1 N9 88.39(2) . 3_577
C3 Co1 N9 173.20(2) . 3_577
C2 Co1 N9 92.45(2) . 3_577
O1 Co1 N9 86.144(19) . 3_577
N4 Co1 N9 95.44(2) . 3_577
O1 Co2 O1 180.0 . 3_577
O1 Co2 N5 82.391(18) . .
O1 Co2 N5 97.609(18) 3_577 .
O1 Co2 N5 97.609(18) . 3_577
O1 Co2 N5 82.391(18) 3_577 3_577
N5 Co2 N5 179.999(9) . 3_577
O1 Co2 N8 96.915(18) . .
O1 Co2 N8 83.085(18) 3_577 .
N5 Co2 N8 93.182(19) . .
N5 Co2 N8 86.818(19) 3_577 .
O1 Co2 N8 83.086(18) . 3_577
O1 Co2 N8 96.914(18) 3_577 3_577
N5 Co2 N8 86.817(19) . 3_577
N5 Co2 N8 93.182(19) 3_577 3_577
N8 Co2 N8 180.0 . 3_577
N1 C1 Co1 178.12(6) . .
N2 C2 Co1 177.00(6) . .
N3 C3 Co1 176.52(6) . .
N4 C4 N6 107.80(5) . .
N4 C4 C5 130.05(5) . .
N6 C4 C5 122.14(5) . .
C4 C5 H5A 108.2(8) . .
C4 C5 H5B 105.2(10) . .
H5A C5 H5B 109.2(13) . .
C4 C5 H5C 109.5(8) . .
H5A C5 H5C 114.4(11) . .
H5B C5 H5C 109.9(12) . .
N5 C6 N6 108.55(5) . .
N5 C6 C7 127.17(5) . .
N6 C6 C7 124.26(5) . .
C6 C7 H7A 108.4(7) . .
C6 C7 H7B 109.8(8) . .
H7A C7 H7B 112.7(11) . .
C6 C7 H7C 108.9(8) . .
H7A C7 H7C 108.0(11) . .
H7B C7 H7C 109.1(12) . .
N8 C8 N10 108.57(5) . .
N8 C8 C9 127.47(5) . .
N10 C8 C9 123.95(5) . .
C8 C9 H9A 109.2(9) . .
C8 C9 H9B 109.9(7) . .
H9A C9 H9B 107.8(11) . .
C8 C9 H9C 108.5(7) . .
H9A C9 H9C 109.6(11) . .
H9B C9 H9C 111.8(10) . .
N9 C10 N10 107.88(5) . .
N9 C10 C11 129.25(6) . .
N10 C10 C11 122.81(5) . .
C10 C11 H11A 109.4(9) . .
C10 C11 H11B 110.2(8) . .
H11A C11 H11B 107.7(12) . .
C10 C11 H11C 109.7(9) . .
H11A C11 H11C 106.6(12) . .
H11B C11 H11C 113.1(11) . .
C4 N4 N5 108.09(5) . .
C4 N4 Co1 133.59(4) . .
N5 N4 Co1 117.46(3) . .
C6 N5 N4 107.83(4) . .
C6 N5 Co2 132.98(4) . .
N4 N5 Co2 116.96(3) . .
C4 N6 C6 107.71(5) . .
C4 N6 N7 123.72(5) . .
C6 N6 N7 128.56(5) . .
N6 N7 H1 106.2(7) . .
N6 N7 H2 108.2(7) . .
H1 N7 H2 110.2(10) . .
C8 N8 N9 107.75(5) . .
C8 N8 Co2 132.57(4) . .
N9 N8 Co2 116.46(3) . .
C10 N9 N8 108.16(5) . .
C10 N9 Co1 133.16(4) . 3_577
N8 N9 Co1 117.59(3) . 3_577
C10 N10 C8 107.63(5) . .
C10 N10 N11 124.37(5) . .
C8 N10 N11 128.00(5) . .
N10 N11 H3 112.0(9) . .
N10 N11 H4 108.6(8) . .
H3 N11 H4 107.8(12) . .
Co1 O1 Co2 114.20(2) . .
Co1 O1 H1A 116.1(9) . .
Co2 O1 H1A 128.9(9) . .
H2A O2 H2B 101.2(15) . .
H3A O3A H3B 94.2(17) . .
H3A O3B H3B 101.5(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 C1 1.8547(6) .
Co1 C3 1.8596(7) .
Co1 C2 1.8821(6) .
Co1 O1 1.9049(4) .
Co1 N4 1.9963(5) .
Co1 N9 2.0019(5) 3_577
Co2 O1 1.9949(4) .
Co2 O1 1.9949(4) 3_577
Co2 N5 2.1224(5) .
Co2 N5 2.1225(5) 3_577
Co2 N8 2.1310(5) .
Co2 N8 2.1310(5) 3_577
C1 N1 1.1573(8) .
C2 N2 1.1585(9) .
C3 N3 1.1559(9) .
C4 N4 1.3233(7) .
C4 N6 1.3590(7) .
C4 C5 1.4787(8) .
C5 H5A 0.949(14) .
C5 H5B 0.913(16) .
C5 H5C 0.929(13) .
C6 N5 1.3115(7) .
C6 N6 1.3591(7) .
C6 C7 1.4816(8) .
C7 H7A 0.936(12) .
C7 H7B 0.918(14) .
C7 H7C 0.937(14) .
C8 N8 1.3116(8) .
C8 N10 1.3620(7) .
C8 C9 1.4808(9) .
C9 H9A 0.919(15) .
C9 H9B 0.960(12) .
C9 H9C 0.991(13) .
C10 N9 1.3218(7) .
C10 N10 1.3597(8) .
C10 C11 1.4799(8) .
C11 H11A 0.925(15) .
C11 H11B 0.976(13) .
C11 H11C 0.892(13) .
N4 N5 1.3823(7) .
N6 N7 1.4015(7) .
N7 H1 0.873(11) .
N7 H2 0.865(12) .
N8 N9 1.3848(7) .
N9 Co1 2.0019(5) 3_577
N10 N11 1.4053(7) .
N11 H3 0.841(14) .
N11 H4 0.873(13) .
O1 H1A 0.719(12) .
O2 H2A 0.921(19) .
O2 H2B 0.903(16) .
O3A H3A 0.901(16) .
O3A H3B 0.768(18) .
O3B H3A 0.793(15) .
O3B H3B 0.790(17) .
