#------------------------------------------------------------------------------
#$Date: 2017-04-04 15:54:25 +0300 (Tue, 04 Apr 2017) $
#$Revision: 194789 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/52/4345230.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_4345230
loop_
_publ_author_name
'Vignesh, Kuduva R.'
'Langley, Stuart K.'
'Murray, Keith S.'
'Rajaraman, Gopalan'
_publ_section_title
;
 Exploring the Influence of Diamagnetic Ions on the Mechanism of
 Magnetization Relaxation in {Co(III)2Ln(III)2} (Ln = Dy, Tb, Ho)
 "Butterfly" Complexes.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2518
_journal_page_last               2532
_journal_paper_doi               10.1021/acs.inorgchem.6b02720
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C42 H52 Co2 N4 O20 Tb2'
_chemical_formula_weight         1368.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.49(3)
_cell_angle_beta                 91.81(3)
_cell_angle_gamma                91.40(3)
_cell_formula_units_Z            1
_cell_length_a                   10.092(2)
_cell_length_b                   10.558(2)
_cell_length_c                   11.080(2)
_cell_measurement_reflns_used    26517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.65
_cell_volume                     1179.6(4)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'scans in phi'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_radiation_source         '3BM1 dipole'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71079
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            26517
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    3.735
_exptl_absorpt_correction_T_max  0.654
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.831
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0194P)²+3.2614P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                5478
_reflns_number_total             5561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02720_si_003.cif
_cod_data_source_block           c:\users\55117655\desktop\co2tb2~1\merged\p-1m
_cod_depositor_comments          'Adding full bibliography for 4345230.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4345230
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Tb1 Tb 0.630882(13) 0.940717(13) 0.881932(12) 0.01631(6) Uani 1 1 d .
Co2 Co 0.38589(4) 1.13143(4) 0.83266(4) 0.01531(9) Uani 1 1 d .
O3 O 0.7079(2) 0.8640(2) 0.6839(2) 0.0258(5) Uani 1 1 d .
O4 O 0.2634(2) 1.0521(2) 0.93460(19) 0.0187(4) Uani 1 1 d .
O6 O 0.5053(2) 1.2226(2) 0.7316(2) 0.0200(4) Uani 1 1 d .
O7 O 0.5169(2) 1.1176(2) 0.96195(19) 0.0175(4) Uani 1 1 d .
O8 O 0.3297(2) 1.2960(2) 0.8830(2) 0.0199(4) Uani 1 1 d .
O1 O 0.4393(2) 0.9722(2) 0.77318(19) 0.0189(4) Uani 1 1 d .
O2 O 0.8590(2) 0.9150(2) 0.8203(2) 0.0232(5) Uani 1 1 d .
O5 O 0.3386(3) 1.2755(2) 1.0852(2) 0.0243(5) Uani 1 1 d .
O9 O 0.6940(2) 1.1181(2) 0.7678(2) 0.0223(4) Uani 1 1 d .
N5 N 0.2454(3) 1.1235(3) 0.7074(2) 0.0204(5) Uani 1 1 d .
O10 O 0.9158(3) 0.8833(3) 0.6350(3) 0.0350(6) Uani 1 1 d .
C7 C 0.6285(3) 1.2040(3) 0.7188(3) 0.0198(6) Uani 1 1 d .
N8 N 0.8306(3) 0.8864(3) 0.7105(3) 0.0239(5) Uani 1 1 d .
C9 C 0.1348(3) 1.0372(4) 0.8818(3) 0.0284(7) Uani 1 1 d .
H9A H 0.0681 1.0572 0.9423 0.034 Uiso 1 1 calc R
H9B H 0.1196 0.9483 0.8549 0.034 Uiso 1 1 calc R
C10 C 0.8019(3) 1.2433(3) 0.5704(3) 0.0246(6) Uani 1 1 d .
H10 H 0.8271 1.1584 0.5838 0.030 Uiso 1 1 calc R
C11 C 0.3134(3) 1.3358(3) 0.9904(3) 0.0207(6) Uani 1 1 d .
C12 C 0.3990(4) 0.9613(3) 0.6500(3) 0.0273(7) Uani 1 1 d .
H12A H 0.4060 0.8725 0.6220 0.033 Uiso 1 1 calc R
H12B H 0.4565 1.0157 0.6003 0.033 Uiso 1 1 calc R
C13 C 0.6983(3) 1.2924(3) 0.6348(3) 0.0209(6) Uani 1 1 d .
C14 C 0.1196(4) 1.1242(4) 0.7755(3) 0.0286(7) Uani 1 1 d .
H14A H 0.0441 1.0948 0.7224 0.034 Uiso 1 1 calc R
H14B H 0.1020 1.2113 0.8037 0.034 Uiso 1 1 calc R
C15 C 0.6625(3) 1.4188(3) 0.6194(3) 0.0262(7) Uani 1 1 d .
C16 C 0.8688(4) 1.3155(4) 0.4873(3) 0.0308(7) Uani 1 1 d .
H16 H 0.9381 1.2803 0.4427 0.037 Uiso 1 1 calc R
C17 C 0.2597(4) 1.4668(3) 0.9994(3) 0.0254(7) Uani 1 1 d .
C18 C 0.2577(4) 1.0023(4) 0.6379(3) 0.0321(8) Uani 1 1 d .
H18A H 0.2330 1.0153 0.5518 0.039 Uiso 1 1 calc R
H18B H 0.1975 0.9362 0.6702 0.039 Uiso 1 1 calc R
C20 C 0.2458(4) 1.2324(3) 0.6247(3) 0.0302(7) Uani 1 1 d .
H20A H 0.1633 1.2309 0.5756 0.045 Uiso 1 1 calc R
H20B H 0.3215 1.2271 0.5718 0.045 Uiso 1 1 calc R
H20C H 0.2529 1.3114 0.6717 0.045 Uiso 1 1 calc R
C22 C 0.1710(4) 1.4993(3) 1.0893(3) 0.0294(7) Uani 1 1 d .
C23 C 0.5573(4) 1.4835(3) 0.6899(4) 0.0336(8) Uani 1 1 d .
H23A H 0.5672 1.5755 0.6812 0.050 Uiso 1 1 calc R
H23B H 0.5671 1.4614 0.7754 0.050 Uiso 1 1 calc R
H23C H 0.4693 1.4556 0.6589 0.050 Uiso 1 1 calc R
C24 C 0.3013(4) 1.5561(3) 0.9158(4) 0.0301(7) Uani 1 1 d .
H24 H 0.3589 1.5317 0.8540 0.036 Uiso 1 1 calc R
C26 C 0.7336(4) 1.4909(4) 0.5365(4) 0.0332(8) Uani 1 1 d .
H26 H 0.7127 1.5774 0.5257 0.040 Uiso 1 1 calc R
C28 C 0.8331(4) 1.4399(4) 0.4701(4) 0.0339(8) Uani 1 1 d .
H28 H 0.8771 1.4903 0.4124 0.041 Uiso 1 1 calc R
C1 C 0.2594(4) 1.6809(3) 0.9216(4) 0.0347(8) Uani 1 1 d .
H1 H 0.2888 1.7417 0.8649 0.042 Uiso 1 1 calc R
C2 C 0.1307(4) 1.6259(4) 1.0929(4) 0.0369(9) Uani 1 1 d .
H2 H 0.0716 1.6509 1.1533 0.044 Uiso 1 1 calc R
C3 C 0.1163(5) 1.4065(4) 1.1785(4) 0.0387(9) Uani 1 1 d .
H3A H 0.1844 1.3894 1.2408 0.058 Uiso 1 1 calc R
H3B H 0.0900 1.3273 1.1364 0.058 Uiso 1 1 calc R
H3C H 0.0389 1.4423 1.2161 0.058 Uiso 1 1 calc R
C4 C 0.1741(4) 1.7148(4) 1.0115(4) 0.0361(9) Uani 1 1 d .
H4 H 0.1454 1.7997 1.0172 0.043 Uiso 1 1 calc R
H7 H 0.566(5) 1.194(5) 0.974(5) 0.043 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'
Tb Tb -0.1723 4.1537 '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
O4 Tb1 O1 147.08(8) 2_677 .
O4 Tb1 O5 79.55(9) 2_677 2_677
O1 Tb1 O5 110.79(9) . 2_677
O4 Tb1 O9 110.06(9) 2_677 .
O1 Tb1 O9 79.60(8) . .
O5 Tb1 O9 145.50(8) 2_677 .
O4 Tb1 O7 69.00(8) 2_677 2_677
O1 Tb1 O7 83.53(8) . 2_677
O5 Tb1 O7 74.13(8) 2_677 2_677
O9 Tb1 O7 140.35(8) . 2_677
O4 Tb1 O7 82.80(8) 2_677 .
O1 Tb1 O7 69.62(8) . .
O5 Tb1 O7 140.99(8) 2_677 .
O9 Tb1 O7 73.42(8) . .
O7 Tb1 O7 67.09(9) 2_677 .
O4 Tb1 O2 80.32(8) 2_677 .
O1 Tb1 O2 131.72(8) . .
O5 Tb1 O2 78.11(9) 2_677 .
O9 Tb1 O2 71.41(8) . .
O7 Tb1 O2 141.57(8) 2_677 .
O7 Tb1 O2 132.45(8) . .
O4 Tb1 O3 130.16(8) 2_677 .
O1 Tb1 O3 82.68(8) . .
O5 Tb1 O3 76.97(9) 2_677 .
O9 Tb1 O3 71.78(9) . .
O7 Tb1 O3 140.88(8) 2_677 .
O7 Tb1 O3 138.65(8) . .
O2 Tb1 O3 52.18(8) . .
O4 Co2 O1 91.23(10) . .
O4 Co2 O6 176.18(10) . .
O1 Co2 O6 92.53(10) . .
O4 Co2 O8 90.84(10) . .
O1 Co2 O8 176.54(10) . .
O6 Co2 O8 85.37(10) . .
O4 Co2 O7 87.66(10) . .
O1 Co2 O7 88.53(10) . .
O6 Co2 O7 93.09(10) . .
O8 Co2 O7 94.33(10) . .
O4 Co2 N5 86.71(11) . .
O1 Co2 N5 86.80(11) . .
O6 Co2 N5 92.84(11) . .
O8 Co2 N5 90.54(11) . .
O7 Co2 N5 172.61(11) . .
O4 Co2 Tb1 42.41(7) . 2_677
O1 Co2 Tb1 98.42(7) . 2_677
O6 Co2 Tb1 137.37(7) . 2_677
O8 Co2 Tb1 84.98(7) . 2_677
O7 Co2 Tb1 46.56(7) . 2_677
N5 Co2 Tb1 128.65(9) . 2_677
N8 O3 Tb1 94.09(18) . .
C9 O4 Co2 113.6(2) . .
C9 O4 Tb1 140.7(2) . 2_677
Co2 O4 Tb1 103.42(10) . 2_677
C7 O6 Co2 127.6(2) . .
Co2 O7 Tb1 97.67(9) . 2_677
Co2 O7 Tb1 97.40(9) . .
Tb1 O7 Tb1 112.91(9) 2_677 .
Co2 O7 H7 112(3) . .
Tb1 O7 H7 116(3) 2_677 .
Tb1 O7 H7 117(3) . .
C11 O8 Co2 127.8(2) . .
C12 O1 Co2 108.51(19) . .
C12 O1 Tb1 135.4(2) . .
Co2 O1 Tb1 102.37(10) . .
N8 O2 Tb1 96.36(18) . .
C11 O5 Tb1 131.4(2) . 2_677
C7 O9 Tb1 132.2(2) . .
C20 N5 C14 108.4(3) . .
C20 N5 C18 110.3(3) . .
C14 N5 C18 111.3(3) . .
C20 N5 Co2 114.2(2) . .
C14 N5 Co2 104.4(2) . .
C18 N5 Co2 108.1(2) . .
O9 C7 O6 125.9(3) . .
O9 C7 C13 118.2(3) . .
O6 C7 C13 116.0(3) . .
O10 N8 O2 121.5(3) . .
O10 N8 O3 122.2(3) . .
O2 N8 O3 116.3(3) . .
O4 C9 C14 109.9(3) . .
O4 C9 H9A 109.7 . .
C14 C9 H9A 109.7 . .
O4 C9 H9B 109.7 . .
C14 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
C16 C10 C13 121.4(3) . .
C16 C10 H10 119.3 . .
C13 C10 H10 119.3 . .
O5 C11 O8 125.7(3) . .
O5 C11 C17 119.4(3) . .
O8 C11 C17 114.9(3) . .
O1 C12 C18 108.0(3) . .
O1 C12 H12A 110.1 . .
C18 C12 H12A 110.1 . .
O1 C12 H12B 110.1 . .
C18 C12 H12B 110.1 . .
H12A C12 H12B 108.4 . .
C10 C13 C15 120.2(3) . .
C10 C13 C7 117.0(3) . .
C15 C13 C7 122.7(3) . .
N5 C14 C9 108.3(3) . .
N5 C14 H14A 110.0 . .
C9 C14 H14A 110.0 . .
N5 C14 H14B 110.0 . .
C9 C14 H14B 110.0 . .
H14A C14 H14B 108.4 . .
C13 C15 C26 117.3(3) . .
C13 C15 C23 124.5(3) . .
C26 C15 C23 118.2(3) . .
C10 C16 C28 118.8(3) . .
C10 C16 H16 120.6 . .
C28 C16 H16 120.6 . .
C24 C17 C22 120.7(3) . .
C24 C17 C11 117.8(3) . .
C22 C17 C11 121.4(3) . .
N5 C18 C12 108.3(3) . .
N5 C18 H18A 110.0 . .
C12 C18 H18A 110.0 . .
N5 C18 H18B 110.0 . .
C12 C18 H18B 110.0 . .
H18A C18 H18B 108.4 . .
N5 C20 H20A 109.5 . .
N5 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
N5 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C17 C22 C2 117.0(4) . .
C17 C22 C3 123.7(3) . .
C2 C22 C3 119.2(3) . .
C15 C23 H23A 109.5 . .
C15 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C15 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C17 C24 C1 120.9(4) . .
C17 C24 H24 119.6 . .
C1 C24 H24 119.6 . .
C28 C26 C15 121.9(3) . .
C28 C26 H26 119.1 . .
C15 C26 H26 119.1 . .
C26 C28 C16 120.3(3) . .
C26 C28 H28 119.9 . .
C16 C28 H28 119.9 . .
C4 C1 C24 118.9(4) . .
C4 C1 H1 120.6 . .
C24 C1 H1 120.6 . .
C4 C2 C22 122.1(4) . .
C4 C2 H2 119.0 . .
C22 C2 H2 119.0 . .
C22 C3 H3A 109.5 . .
C22 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C22 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 C1 120.3(3) . .
C2 C4 H4 119.8 . .
C1 C4 H4 119.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O4 2.266(2) 2_677
Tb1 O1 2.278(2) .
Tb1 O5 2.341(2) 2_677
Tb1 O9 2.355(2) .
Tb1 O7 2.394(2) 2_677
Tb1 O7 2.395(2) .
Tb1 O2 2.443(2) .
Tb1 O3 2.487(2) .
Co2 O4 1.887(2) .
Co2 O1 1.897(2) .
Co2 O6 1.918(2) .
Co2 O8 1.925(2) .
Co2 O7 1.927(2) .
Co2 N5 1.952(3) .
Co2 Tb1 3.2676(8) 2_677
O3 N8 1.280(4) .
O4 C9 1.410(4) .
O4 Tb1 2.266(2) 2_677
O6 C7 1.276(4) .
O7 Tb1 2.394(2) 2_677
O7 H7 0.94(5) .
O8 C11 1.275(4) .
O1 C12 1.415(4) .
O2 N8 1.273(4) .
O5 C11 1.256(4) .
O5 Tb1 2.341(2) 2_677
O9 C7 1.252(4) .
N5 C20 1.476(4) .
N5 C14 1.497(4) .
N5 C18 1.498(4) .
O10 N8 1.220(4) .
C7 C13 1.503(4) .
C9 C14 1.507(5) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C16 1.382(5) .
C10 C13 1.392(5) .
C10 H10 0.9500 .
C11 C17 1.501(4) .
C12 C18 1.502(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C15 1.402(5) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C26 1.402(5) .
C15 C23 1.511(5) .
C16 C28 1.383(6) .
C16 H16 0.9500 .
C17 C24 1.394(5) .
C17 C22 1.406(5) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C22 C2 1.407(5) .
C22 C3 1.506(6) .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 C1 1.395(5) .
C24 H24 0.9500 .
C26 C28 1.381(6) .
C26 H26 0.9500 .
C28 H28 0.9500 .
C1 C4 1.388(6) .
C1 H1 0.9500 .
C2 C4 1.381(6) .
C2 H2 0.9500 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4 0.9500 .
