#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:37:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179453 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/50/4335007.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_4335007
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Sakiat Hossain'
'Sourav Das'
'Sourav Biswas'
'Jean-Pascal Sutter'
_publ_section_title
;
 Rhombus-Shaped Tetranuclear [Ln4] Complexes [Ln = Dy(III) and Ho(III)]:
 Synthesis, Structure, and SMM Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6346
_journal_page_last               6353
_journal_paper_doi               10.1021/ic302848k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C34 H22 Ho4 N8 O18, 6(CH3OH), 4(H2O)'
_chemical_formula_sum            'C40 H54 Ho4 N8 O28'
_chemical_formula_weight         1754.03
_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                105.040(6)
_cell_angle_beta                 91.041(7)
_cell_angle_gamma                104.007(7)
_cell_formula_units_Z            1
_cell_length_a                   10.431(4)
_cell_length_b                   11.430(4)
_cell_length_c                   11.838(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1317.6(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_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            7042
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    6.037
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.733
_refine_diff_density_min         -3.028
_refine_diff_density_rms         0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4809
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1596P)²+20.7035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2797
_reflns_number_gt                3116
_reflns_number_total             4809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302848k_si_001_2.cif
_cod_data_source_block           Complex2
_cod_database_code               4335007
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
Ho4 Ho 0.13101(10) 0.64757(9) 0.27260(8) 0.0267(3) Uani 1 1 d .
Ho3 Ho -0.03229(14) 0.35172(10) 0.03615(9) 0.0441(4) Uani 1 1 d .
O19 O 0.4802(9) 0.8592(9) 0.9682(10) 0.005(2) Uani 1 1 d U
N6 N 0.1096(16) 0.4165(15) 0.4137(14) 0.022(2) Uani 1 1 d .
O15 O 0.6944(11) 0.6118(11) 0.1971(10) 0.010(2) Uani 1 1 d .
N8 N 0.1599(16) 0.5436(15) 0.4358(14) 0.022(2) Uani 1 1 d .
O17 O 0.4809(11) 0.4567(11) 0.3993(10) 0.010(2) Uani 1 1 d U
O13 O 0.0524(12) 0.4291(12) 0.2338(12) 0.022(3) Uani 1 1 d U
O12 O 0.1910(13) 0.8553(13) 0.2738(12) 0.025(3) Uani 1 1 d U
O16 O 0.5480(11) 0.6769(11) 0.0968(10) 0.012(2) Uani 1 1 d U
O18 O 0.6732(18) 0.7357(16) 0.8130(17) 0.050(5) Uani 1 1 d .
C25 C 0.2213(19) 0.6095(18) 0.5344(18) 0.022(4) Uani 1 1 d U
H25 H 0.2360 0.5714 0.5922 0.027 Uiso 1 1 calc R
O14 O -0.1366(16) 0.1463(13) -0.0676(12) 0.033(4) Uani 1 1 d .
C28 C 0.353(2) 0.9978(19) 0.5736(17) 0.022(4) Uani 1 1 d .
C24 C 0.063(2) 0.369(2) 0.3080(19) 0.026(4) Uani 1 1 d U
C27 C 0.2825(19) 0.9096(19) 0.4725(18) 0.023(4) Uani 1 1 d U
C31 C 0.394(2) 1.129(2) 0.574(2) 0.036(5) Uani 1 1 d U
H31 H 0.4441 1.1895 0.6382 0.044 Uiso 1 1 calc R
N5 N -0.0507(17) 0.1958(18) 0.1509(15) 0.029(4) Uani 1 1 d .
C23 C -0.1242(19) -0.0162(19) 0.1635(18) 0.023(4) Uani 1 1 d U
H23 H -0.1666 -0.0999 0.1287 0.027 Uiso 1 1 calc R
C29 C 0.382(2) 0.951(2) 0.668(2) 0.031(5) Uani 1 1 d .
H29 H 0.4299 1.0046 0.7372 0.037 Uiso 1 1 calc R
N7 N 0.2392(17) 0.7861(16) 0.4626(16) 0.028(4) Uani 1 1 d .
C18 C -0.1716(18) 0.0404(18) -0.0238(17) 0.020(4) Uani 1 1 d U
H18A H -0.1377 -0.0264 -0.0716 0.024 Uiso 1 1 calc R
H18B H -0.2674 0.0110 -0.0286 0.024 Uiso 1 1 calc R
C36 C 0.417(3) 0.607(3) 0.040(3) 0.077(10) Uani 1 1 d U
H36A H 0.3517 0.6144 0.0959 0.115 Uiso 1 1 calc R
H36B H 0.4153 0.5202 0.0088 0.115 Uiso 1 1 calc R
H36C H 0.3961 0.6399 -0.0232 0.115 Uiso 1 1 calc R
C20 C -0.0002(19) 0.2324(19) 0.2622(18) 0.023(4) Uani 1 1 d U
C35 C 0.697(4) 0.556(3) 0.253(3) 0.074(10) Uani 1 1 d .
C32 C 0.356(2) 1.159(2) 0.4783(19) 0.027(5) Uani 1 1 d U
H32 H 0.3754 1.2430 0.4803 0.033 Uiso 1 1 calc R
C22 C -0.070(2) 0.018(2) 0.2774(18) 0.028(5) Uani 1 1 d .
H22 H -0.0769 -0.0409 0.3199 0.034 Uiso 1 1 calc R
C30 C 0.3381(18) 0.8221(18) 0.6574(17) 0.021(4) Uani 1 1 d .
H30 H 0.3569 0.7916 0.7197 0.025 Uiso 1 1 calc R
C34 C 0.253(2) 0.946(2) 0.3709(18) 0.026(3) Uani 1 1 d .
C33 C 0.2883(19) 1.0718(19) 0.3758(19) 0.026(3) Uani 1 1 d U
H33 H 0.2676 1.0986 0.3116 0.031 Uiso 1 1 calc R
C26 C 0.2660(19) 0.7377(19) 0.5547(18) 0.025(4) Uani 1 1 d U
C19 C -0.1179(19) 0.070(2) 0.0979(17) 0.024(4) Uani 1 1 d .
C21 C -0.004(2) 0.1457(19) 0.3289(19) 0.027(5) Uani 1 1 d U
H21 H 0.0363 0.1718 0.4051 0.032 Uiso 1 1 calc R
O20 O 0.162(3) 0.587(3) 0.077(3) 0.115(10) Uani 1 1 d U
O22 O 0.037(4) 0.386(4) -0.135(3) 0.145(13) Uani 1 1 d U
O27 O -0.0548(13) 0.6628(13) 0.3801(13) 0.028(3) Uani 1 1 d .
O31 O 0.3469(14) 0.6198(16) 0.2679(13) 0.044(5) Uani 1 1 d .
O26 O -0.2326(18) 0.3479(16) 0.1343(15) 0.045(4) Uani 1 1 d .
O30 O 0.177(2) 0.3083(16) 0.0293(16) 0.056(6) Uani 1 1 d .
C37 C 0.476(3) 0.495(3) 0.341(3) 0.066(9) Uani 1 1 d .
H37A H 0.4188 0.5495 0.3600 0.099 Uiso 1 1 calc R
H37B H 0.4425 0.4320 0.2683 0.099 Uiso 1 1 calc R
H37C H 0.5636 0.5422 0.3326 0.099 Uiso 1 1 calc 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'
Ho Ho -0.2175 4.6783 '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'
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
O22 Ho4 O20 59.5(11) 2_565 .
O22 Ho4 O12 89.3(10) 2_565 .
O20 Ho4 O12 91.0(9) . .
O22 Ho4 O31 134.7(10) 2_565 .
O20 Ho4 O31 75.4(8) . .
O12 Ho4 O31 95.9(5) . .
O22 Ho4 O13 80.7(10) 2_565 .
O20 Ho4 O13 79.7(9) . .
O12 Ho4 O13 168.8(5) . .
O31 Ho4 O13 87.8(5) . .
O22 Ho4 O27 75.5(10) 2_565 .
O20 Ho4 O27 134.5(8) . .
O12 Ho4 O27 95.2(5) . .
O31 Ho4 O27 147.8(6) . .
O13 Ho4 O27 87.1(4) . .
O22 Ho4 N7 143.5(10) 2_565 .
O20 Ho4 N7 142.9(9) . .
O12 Ho4 N7 67.2(5) . .
O31 Ho4 N7 77.4(5) . .
O13 Ho4 N7 124.0(5) . .
O27 Ho4 N7 79.3(5) . .
O22 Ho4 N8 132.8(10) 2_565 .
O20 Ho4 N8 130.1(8) . .
O12 Ho4 N8 130.2(5) . .
O31 Ho4 N8 73.8(6) . .
O13 Ho4 N8 61.0(5) . .
O27 Ho4 N8 76.0(5) . .
N7 Ho4 N8 63.0(5) . .
O22 Ho4 Ho3 50.9(9) 2_565 .
O20 Ho4 Ho3 49.2(8) . .
O12 Ho4 Ho3 132.5(4) . .
O31 Ho4 Ho3 96.9(4) . .
O13 Ho4 Ho3 36.3(3) . .
O27 Ho4 Ho3 97.6(3) . .
N7 Ho4 Ho3 160.3(4) . .
N8 Ho4 Ho3 97.3(4) . .
O22 Ho4 Ho3 33.2(9) 2_565 2_565
O20 Ho4 Ho3 32.7(7) . 2_565
O12 Ho4 Ho3 75.3(4) . 2_565
O31 Ho4 Ho3 105.4(4) . 2_565
O13 Ho4 Ho3 93.5(3) . 2_565
O27 Ho4 Ho3 106.6(4) . 2_565
N7 Ho4 Ho3 142.4(4) . 2_565
N8 Ho4 Ho3 154.5(4) . 2_565
Ho3 Ho4 Ho3 57.18(4) . 2_565
O20 Ho3 O22 60.5(12) 2_565 .
O20 Ho3 O14 87.3(9) 2_565 .
O22 Ho3 O14 88.2(10) . .
O20 Ho3 O13 133.6(8) 2_565 .
O22 Ho3 O13 135.2(10) . .
O14 Ho3 O13 128.5(5) . .
O20 Ho3 O30 136.7(9) 2_565 .
O22 Ho3 O30 76.2(10) . .
O14 Ho3 O30 91.7(6) . .
O13 Ho3 O30 77.8(5) . .
O20 Ho3 O26 75.7(9) 2_565 .
O22 Ho3 O26 136.1(10) . .
O14 Ho3 O26 85.7(6) . .
O13 Ho3 O26 78.6(5) . .
O30 Ho3 O26 147.3(6) . .
O20 Ho3 N5 139.2(9) 2_565 .
O22 Ho3 N5 140.9(10) . .
O14 Ho3 N5 65.1(5) . .
O13 Ho3 N5 63.4(5) . .
O30 Ho3 N5 76.5(6) . .
O26 Ho3 N5 72.9(5) . .
O20 Ho3 O20 90.5(10) 2_565 .
O22 Ho3 O20 69.2(11) . .
O14 Ho3 O20 155.0(7) . .
O13 Ho3 O20 68.6(7) . .
O30 Ho3 O20 73.1(7) . .
O26 Ho3 O20 117.9(7) . .
N5 Ho3 O20 127.2(8) . .
O20 Ho3 Ho3 52.4(8) 2_565 2_565
O22 Ho3 Ho3 54.2(9) . 2_565
O14 Ho3 Ho3 133.6(3) . 2_565
O13 Ho3 Ho3 97.8(3) . 2_565
O30 Ho3 Ho3 102.6(4) . 2_565
O26 Ho3 Ho3 102.6(4) . 2_565
N5 Ho3 Ho3 161.1(4) . 2_565
O20 Ho3 Ho3 38.0(6) . 2_565
O20 Ho3 Ho4 104.4(8) 2_565 .
O22 Ho3 Ho4 106.0(10) . .
O14 Ho3 Ho4 164.8(3) . .
O13 Ho3 Ho4 36.4(3) . .
O30 Ho3 Ho4 86.4(4) . .
O26 Ho3 Ho4 87.8(4) . .
N5 Ho3 Ho4 99.8(4) . .
O20 Ho3 Ho4 37.2(6) . .
Ho3 Ho3 Ho4 61.42(4) 2_565 .
O20 Ho3 Ho4 33.7(8) 2_565 2_565
O22 Ho3 Ho4 33.4(9) . 2_565
O14 Ho3 Ho4 72.2(3) . 2_565
O13 Ho3 Ho4 159.2(3) . 2_565
O30 Ho3 Ho4 105.7(4) . 2_565
O26 Ho3 Ho4 104.4(4) . 2_565
N5 Ho3 Ho4 137.4(4) . 2_565
O20 Ho3 Ho4 92.5(6) . 2_565
Ho3 Ho3 Ho4 61.40(3) 2_565 2_565
Ho4 Ho3 Ho4 122.82(4) . 2_565
C24 N6 N8 110.4(17) . .
C25 N8 N6 121.3(17) . .
C25 N8 Ho4 120.1(14) . .
N6 N8 Ho4 118.6(11) . .
C24 O13 Ho3 129.0(13) . .
C24 O13 Ho4 123.7(13) . .
Ho3 O13 Ho4 107.3(5) . .
C34 O12 Ho4 121.4(12) . .
N8 C25 C26 120(2) . .
C18 O14 Ho3 127.7(12) . .
C27 C28 C29 116.7(19) . .
C27 C28 C31 118.8(18) . .
C29 C28 C31 124(2) . .
N6 C24 O13 126(2) . .
N6 C24 C20 121(2) . .
O13 C24 C20 112.6(18) . .
N7 C27 C28 123.9(19) . .
N7 C27 C34 114.7(19) . .
C28 C27 C34 121.4(19) . .
C32 C31 C28 117(2) . .
C20 N5 C19 120.9(18) . .
C20 N5 Ho3 119.8(14) . .
C19 N5 Ho3 119.2(13) . .
C22 C23 C19 122(2) . .
C30 C29 C28 119(2) . .
C27 N7 C26 120.5(18) . .
C27 N7 Ho4 118.1(14) . .
C26 N7 Ho4 121.2(13) . .
O14 C18 C19 111.0(16) . .
N5 C20 C21 121.5(19) . .
N5 C20 C24 114.9(19) . .
C21 C20 C24 123.6(19) . .
C31 C32 C33 125(2) . .
C23 C22 C21 118(2) . .
C29 C30 C26 121.9(19) . .
O12 C34 C33 123.1(19) . .
O12 C34 C27 118.6(19) . .
C33 C34 C27 118(2) . .
C34 C33 C32 119(2) . .
C25 C26 N7 116.0(19) . .
C25 C26 C30 126(2) . .
N7 C26 C30 117.8(18) . .
C23 C19 N5 118.0(18) . .
C23 C19 C18 125.5(19) . .
N5 C19 C18 116.5(18) . .
C20 C21 C22 119(2) . .
Ho3 O20 Ho4 113.6(12) 2_565 .
Ho3 O20 Ho3 89.5(10) 2_565 .
Ho4 O20 Ho3 93.6(10) . .
Ho3 O22 Ho4 113.4(15) . 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho4 O22 2.27(4) 2_565
Ho4 O20 2.29(3) .
Ho4 O12 2.300(14) .
Ho4 O31 2.349(15) .
Ho4 O13 2.349(13) .
Ho4 O27 2.354(13) .
Ho4 N7 2.456(18) .
Ho4 N8 2.564(16) .
Ho4 Ho3 3.7812(17) .
Ho4 Ho3 3.7817(19) 2_565
Ho3 O20 2.23(3) 2_565
Ho3 O22 2.26(4) .
Ho3 O14 2.329(15) .
Ho3 O13 2.347(14) .
Ho3 O30 2.35(2) .
Ho3 O26 2.406(19) .
Ho3 N5 2.482(18) .
Ho3 O20 2.87(3) .
Ho3 Ho3 3.619(2) 2_565
Ho3 Ho4 3.7817(19) 2_565
N6 C24 1.26(3) .
N6 N8 1.37(2) .
O15 C35 1.04(4) .
N8 C25 1.27(3) .
O17 C37 0.91(3) .
O13 C24 1.26(2) .
O12 C34 1.36(2) .
O16 C36 1.46(4) .
C25 C26 1.38(3) .
O14 C18 1.41(2) .
C28 C27 1.41(3) .
C28 C29 1.42(3) .
C28 C31 1.45(3) .
C24 C20 1.49(3) .
C27 N7 1.35(3) .
C27 C34 1.42(3) .
C31 C32 1.35(3) .
N5 C20 1.33(3) .
N5 C19 1.41(3) .
C23 C22 1.37(3) .
C23 C19 1.40(3) .
C29 C30 1.40(3) .
N7 C26 1.40(3) .
C18 C19 1.46(3) .
C20 C21 1.41(3) .
C32 C33 1.40(3) .
C22 C21 1.42(3) .
C30 C26 1.41(3) .
C34 C33 1.38(3) .
O20 Ho3 2.23(3) 2_565
O22 Ho4 2.27(4) 2_565
