#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/80/4328072.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_4328072
loop_
_publ_author_name
'George J. Sopasis'
'Maria Orfanoudaki'
'Pavlos Zarmpas'
'Aggelos Philippidis'
'Milosz Siczek'
'Tadeusz Lis'
'James R. O'Brien'
'Constantinos J. Milios'
_publ_section_title
;
 2-Aminoisobutyric Acid in Co(II) and Co(II)/Ln(III) Chemistry:
 Homometallic and Heterometallic Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1170
_journal_page_last               1179
_journal_paper_doi               10.1021/ic2024007
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C24 H63 Co6 N9 O30 Tm, 1.48(Cl O4), 1.52(N O3), 3(H2 O)'
_chemical_formula_sum            'C24 H69 Cl1.48 Co6 N10.52 O43.48 Tm'
_chemical_formula_weight         1775.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.453(4)
_cell_length_b                   12.453(4)
_cell_length_c                   22.078(8)
_cell_measurement_reflns_used    3510
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.6
_cell_volume                     2965.1(17)
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Xcalibur PX KM4CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.1143
_diffrn_reflns_av_sigmaI/netI    0.1551
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22347
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    3.299
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_description       block
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0342
_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/[σ²(Fo²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0336
_refine_ls_wR_factor_ref         0.0362
_reflns_number_gt                1588
_reflns_number_total             2930
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2024007_si_002_11.cif
_cod_data_source_block           complex_13
_cod_original_sg_symbol_Hall     '-P 6c '
_cod_database_code               4328072
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
Tm Tm 0.6667 0.3333 0.2500 0.01437(10) Uani 1 6 d S
Co Co 0.88420(4) 0.28011(4) 0.326128(19) 0.01655(11) Uani 1 1 d .
O1 O 0.6410(2) 0.5073(2) 0.2500 0.0119(7) Uani 1 2 d S
H1 H 0.5505 0.4798 0.2500 0.014 Uiso 1 2 calc SR
O11 O 0.69251(17) 0.21148(17) 0.32846(9) 0.0144(5) Uani 1 1 d .
O21 O 0.51664(18) 0.08553(18) 0.37888(9) 0.0200(6) Uani 1 1 d .
N11 N 0.8320(2) 0.1501(2) 0.39505(10) 0.0277(7) Uani 1 1 d .
H11A H 0.8414 0.0853 0.3816 0.033 Uiso 1 1 calc R
H11B H 0.8847 0.1859 0.4274 0.033 Uiso 1 1 calc R
C11 C 0.6317(3) 0.1346(3) 0.37074(14) 0.0175(8) Uani 1 1 d .
C21 C 0.7025(3) 0.1000(3) 0.41621(15) 0.0210(8) Uani 1 1 d .
C31 C 0.7029(3) 0.1588(3) 0.47632(14) 0.0370(10) Uani 1 1 d .
H31A H 0.7421 0.1331 0.5072 0.055 Uiso 1 1 calc R
H31B H 0.6174 0.1319 0.4884 0.055 Uiso 1 1 calc R
H31C H 0.7494 0.2492 0.4723 0.055 Uiso 1 1 calc R
C41 C 0.6379(3) -0.0396(3) 0.42330(15) 0.0362(11) Uani 1 1 d .
H41A H 0.6364 -0.0775 0.3842 0.054 Uiso 1 1 calc R
H41B H 0.5528 -0.0705 0.4374 0.054 Uiso 1 1 calc R
H41C H 0.6828 -0.0610 0.4529 0.054 Uiso 1 1 calc R
O1W O 1.06852(17) 0.33789(17) 0.32853(9) 0.0300(6) Uani 1 1 d .
H1W1 H 1.0958 0.2917 0.3170 0.045 Uiso 1 1 d R
H1W2 H 1.1219 0.4120 0.3356 0.045 Uiso 1 1 d R
Cl1 Cl 0.0000 0.0000 0.5000 0.0331(6) Uani 1 6 d S
O2 O 0.1177(4) 0.0884(5) 0.5175(3) 0.0485(16) Uani 0.50 1 d P
O3 O 0.0000 0.0000 0.5674(4) 0.072(3) Uani 0.50 3 d SP
N1 N 0.8339(4) 0.0310(4) 0.2500 0.0255(11) Uani 1 2 d S
O4 O 0.8178(2) -0.0228(2) 0.29933(11) 0.0425(8) Uani 1 1 d .
O5 O 0.8701(2) 0.1476(3) 0.2500 0.0222(8) Uani 1 2 d S
Cl2 Cl 0.6667 0.3333 0.6408(4) 0.0197(18) Uani 0.24 3 d SP
O7 O 0.6667 0.3333 0.5822(11) 0.105(8) Uiso 0.24 3 d SP
N2 N 0.6667 0.3333 0.6655(4) 0.039(4) Uiso 0.76 3 d SP
O6 O 0.5921(2) 0.3740(2) 0.66270(13) 0.0637(9) Uani 1 1 d .
O2W O 0.3846(3) 0.4450(3) 0.2500 0.0408(10) Uani 1 2 d S
H2W H 0.3840 0.4833 0.2813 0.061 Uiso 1 1 d R
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'
Cl Cl 0.1484 0.1585 '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'
Tm Tm -0.3139 5.2483 '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
O1 Tm O1 120.0 . 3_665
O1 Tm O1 120.0 . 2_655
O1 Tm O11 71.21(6) . 12_666
O1 Tm O11 134.42(5) 3_665 12_666
O1 Tm O11 67.80(6) 2_655 12_666
O1 Tm O11 71.21(6) . 3_665
O1 Tm O11 134.42(5) 3_665 3_665
O1 Tm O11 67.80(6) 2_655 3_665
O11 Tm O11 91.03(9) 12_666 3_665
O1 Tm O11 134.42(5) . 10_556
O1 Tm O11 67.80(6) 3_665 10_556
O1 Tm O11 71.21(6) 2_655 10_556
O11 Tm O11 74.72(7) 12_666 10_556
O11 Tm O11 138.98(4) 3_665 10_556
O1 Tm O11 134.42(5) . .
O1 Tm O11 67.80(6) 3_665 .
O1 Tm O11 71.21(6) 2_655 .
O11 Tm O11 138.98(4) 12_666 .
O11 Tm O11 74.72(7) 3_665 .
O11 Tm O11 91.03(9) 10_556 .
O1 Tm O11 67.80(6) . 2_655
O1 Tm O11 71.21(6) 3_665 2_655
O1 Tm O11 134.42(5) 2_655 2_655
O11 Tm O11 138.98(4) 12_666 2_655
O11 Tm O11 74.72(7) 3_665 2_655
O11 Tm O11 138.98(4) 10_556 2_655
O11 Tm O11 74.72(7) . 2_655
O1 Tm O11 67.80(6) . 11_656
O1 Tm O11 71.21(6) 3_665 11_656
O1 Tm O11 134.42(5) 2_655 11_656
O11 Tm O11 74.72(7) 12_666 11_656
O11 Tm O11 138.98(4) 3_665 11_656
O11 Tm O11 74.72(7) 10_556 11_656
O11 Tm O11 138.98(4) . 11_656
O11 Tm O11 91.03(9) 2_655 11_656
O1 Co O1W 103.25(9) 3_665 .
O1 Co N11 157.59(10) 3_665 .
O1W Co N11 96.57(9) . .
O1 Co O21 92.32(9) 3_665 2_655
O1W Co O21 90.19(8) . 2_655
N11 Co O21 98.02(9) . 2_655
O1 Co O11 80.71(9) 3_665 .
O1W Co O11 175.93(8) . .
N11 Co O11 79.37(9) . .
O21 Co O11 90.55(7) 2_655 .
O1 Co O5 75.68(8) 3_665 .
O1W Co O5 86.60(8) . .
N11 Co O5 95.40(9) . .
O21 Co O5 166.47(8) 2_655 .
O11 Co O5 93.58(9) . .
Co O1 Co 113.09(12) 2_655 11_656
Co O1 Tm 107.56(8) 2_655 .
Co O1 Tm 107.56(8) 11_656 .
Co O1 H1 109.5 2_655 .
Co O1 H1 109.5 11_656 .
Tm O1 H1 109.5 . .
C11 O11 Co 116.80(19) . .
C11 O11 Tm 140.74(19) . .
Co O11 Tm 101.98(8) . .
C11 O21 Co 125.6(2) . 3_665
C21 N11 Co 114.12(19) . .
C21 N11 H11A 108.7 . .
Co N11 H11A 108.7 . .
C21 N11 H11B 108.7 . .
Co N11 H11B 108.7 . .
H11A N11 H11B 107.6 . .
O21 C11 O11 124.9(3) . .
O21 C11 C21 116.5(3) . .
O11 C11 C21 118.6(3) . .
N11 C21 C31 109.5(3) . .
N11 C21 C41 110.9(3) . .
C31 C21 C41 109.6(3) . .
N11 C21 C11 109.5(3) . .
C31 C21 C11 107.5(3) . .
C41 C21 C11 109.9(3) . .
C21 C31 H31A 109.5 . .
C21 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C21 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C21 C41 H41A 109.5 . .
C21 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C21 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
Co O1W H1W1 121.4 . .
Co O1W H1W2 121.8 . .
H1W1 O1W H1W2 116.1 . .
O2 Cl1 O2 67.5(2) 3 7_556
O2 Cl1 O2 67.5(2) 3 8_556
O2 Cl1 O2 112.5(2) 7_556 8_556
O2 Cl1 O2 112.5(2) 3 .
O2 Cl1 O2 179.997(1) 7_556 .
O2 Cl1 O2 67.5(2) 8_556 .
O2 Cl1 O2 180.00(15) 3 9_556
O2 Cl1 O2 112.5(2) 7_556 9_556
O2 Cl1 O2 112.5(2) 8_556 9_556
O2 Cl1 O2 67.5(2) . 9_556
O2 Cl1 O2 112.5(2) 3 2
O2 Cl1 O2 67.5(2) 7_556 2
O2 Cl1 O2 180.0(4) 8_556 2
O2 Cl1 O2 112.5(2) . 2
O2 Cl1 O2 67.5(2) 9_556 2
O2 Cl1 O3 73.7(2) 3 .
O2 Cl1 O3 106.3(2) 7_556 .
O2 Cl1 O3 106.3(2) 8_556 .
O2 Cl1 O3 73.7(2) . .
O2 Cl1 O3 106.3(2) 9_556 .
O2 Cl1 O3 73.7(2) 2 .
O2 Cl1 O3 106.3(2) 3 7_556
O2 Cl1 O3 73.7(2) 7_556 7_556
O2 Cl1 O3 73.7(2) 8_556 7_556
O2 Cl1 O3 106.3(2) . 7_556
O2 Cl1 O3 73.7(2) 9_556 7_556
O2 Cl1 O3 106.3(2) 2 7_556
O3 Cl1 O3 180.0 . 7_556
Cl1 O2 O2 56.23(10) . 9_556
Cl1 O2 O2 56.23(10) . 8_556
O2 O2 O2 96.8(5) 9_556 8_556
Cl1 O2 O3 56.1(3) . .
O2 O2 O3 89.5(3) 9_556 .
O2 O2 O3 89.5(3) 8_556 .
Cl1 O3 O2 50.2(3) . .
Cl1 O3 O2 50.2(3) . 3
O2 O3 O2 83.4(4) . 3
Cl1 O3 O2 50.2(3) . 2
O2 O3 O2 83.4(4) . 2
O2 O3 O2 83.4(4) 3 2
O4 N1 O4 122.6(4) 10_556 .
O4 N1 O5 118.7(2) 10_556 .
O4 N1 O5 118.7(2) . .
N1 O5 Co 131.87(7) . 10_556
N1 O5 Co 131.87(7) . .
Co O5 Co 93.93(11) 10_556 .
N2 Cl2 O7 180.000(17) . .
N2 Cl2 O6 69.0(4) . 3_665
O7 Cl2 O6 111.0(4) . 3_665
N2 Cl2 O6 69.0(4) . 2_655
O7 Cl2 O6 111.0(4) . 2_655
O6 Cl2 O6 107.9(4) 3_665 2_655
N2 Cl2 O6 69.0(4) . .
O7 Cl2 O6 111.0(4) . .
O6 Cl2 O6 107.9(4) 3_665 .
O6 Cl2 O6 107.9(4) 2_655 .
Cl2 N2 O6 87.2(4) . 3_665
Cl2 N2 O6 87.2(4) . 2_655
O6 N2 O6 119.77(8) 3_665 2_655
Cl2 N2 O6 87.2(4) . .
O6 N2 O6 119.77(8) 3_665 .
O6 N2 O6 119.77(8) 2_655 .
O6 N2 O7 87.2(4) 3_665 .
O6 N2 O7 87.2(4) 2_655 .
O6 N2 O7 87.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tm O1 2.343(3) .
Tm O11 2.428(2) .
Co O1W 2.0342(19) .
Co N11 2.076(2) .
Co O21 2.080(2) 2_655
Co O11 2.096(2) .
Co O5 2.299(2) .
O1 Co 2.0145(15) 2_655
O1 H1 1.0000 .
O11 C11 1.279(3) .
O21 C11 1.258(3) .
O21 Co 2.080(2) 3_665
N11 C21 1.484(4) .
N11 H11A 0.9200 .
N11 H11B 0.9200 .
C11 C21 1.534(4) .
C21 C31 1.514(4) .
C21 C41 1.515(4) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
O1W H1W1 0.8400 .
O1W H1W2 0.8392 .
Cl1 O2 1.376(4) .
Cl1 O3 1.488(9) .
O2 O2 1.530(6) 9_556
O2 O3 1.721(7) .
N1 O4 1.242(2) .
N1 O5 1.288(4) .
O5 Co 2.299(2) 10_556
Cl2 N2 0.545(14) .
Cl2 O7 1.29(2) .
Cl2 O6 1.351(4) .
O7 N2 1.84(2) .
N2 O6 1.263(2) .
O2W H2W 0.8409 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O2W 1.00 1.89 2.884(4) 174.2 .
N11 H11A O4 0.92 2.19 2.958(4) 140.2 .
O1W H1W1 O4 0.84 1.93 2.765(3) 174.1 3_765
O1W H1W2 O6 0.84 1.94 2.762(3) 164.7 9_656
O2W H2W O6 0.84 2.06 2.868(3) 160.6 7_666
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 Co N11 C21 -38.6(4) 3_665 .
O21 Co N11 C21 78.1(2) 2_655 .
O11 Co N11 C21 -10.9(2) . .
O5 Co N11 C21 -103.6(2) . .
Co O21 C11 O11 0.1(4) 3_665 .
Co O21 C11 C21 178.95(19) 3_665 .
Co O11 C11 O21 179.4(2) . .
Tm O11 C11 O21 9.3(5) . .
Co O11 C11 C21 0.6(3) . .
Tm O11 C11 C21 -169.5(2) . .
Co N11 C21 C31 -103.8(2) . .
Co N11 C21 C41 135.2(2) . .
Co N11 C21 C11 13.8(3) . .
O21 C11 C21 N11 171.6(3) . .
O11 C11 C21 N11 -9.6(4) . .
O21 C11 C21 C31 -69.6(3) . .
O11 C11 C21 C31 109.3(3) . .
O21 C11 C21 C41 49.6(4) . .
O11 C11 C21 C41 -131.5(3) . .
O4 N1 O5 Co 11.4(6) 10_556 10_556
O4 N1 O5 Co -169.3(2) . 10_556
O4 N1 O5 Co 169.3(2) 10_556 .
O4 N1 O5 Co -11.4(6) . .
O1 Co O5 N1 -155.0(3) 3_665 .
O1W Co O5 N1 100.4(3) . .
N11 Co O5 N1 4.2(3) . .
O21 Co O5 N1 177.0(3) 2_655 .
O11 Co O5 N1 -75.5(3) . .
O1 Co O5 Co 8.77(9) 3_665 10_556
O1W Co O5 Co -95.84(9) . 10_556
N11 Co O5 Co 167.87(10) . 10_556
O21 Co O5 Co -19.3(4) 2_655 10_556
O11 Co O5 Co 88.23(9) . 10_556
