#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:37:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179453 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/50/4335006.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_4335006
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 H24 Dy4 N8 O18, 4(C H4 O), 6(O)'
_chemical_formula_sum            'C38 H40 Dy4 N8 O28'
_chemical_formula_weight         1706.78
_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                104.585(5)
_cell_angle_beta                 91.466(5)
_cell_angle_gamma                104.431(5)
_cell_formula_units_Z            1
_cell_length_a                   10.552(5)
_cell_length_b                   11.547(5)
_cell_length_c                   11.927(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1356.0(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       '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      293(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     0.71069
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7296
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    5.541
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.119370
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.858
_refine_diff_density_min         -2.766
_refine_diff_density_rms         0.377
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4945
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0703
_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)+(0.1493P)²+13.7705P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2365
_reflns_number_gt                3914
_reflns_number_total             4945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302848k_si_001_1.cif
_cod_data_source_block           Complex1
_cod_database_code               4335006
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
Dy1 Dy 0.36829(6) 0.35301(5) 0.22883(5) 0.037 Uani 1 1 d .
Dy2 Dy 0.53225(8) 0.64732(5) 0.46286(5) 0.053 Uani 1 1 d .
O1 O 0.6336(11) 0.8538(9) 0.5666(8) 0.050 Uani 1 1 d D
O2 O 0.4466(8) 0.5726(8) 0.2688(7) 0.035 Uani 1 1 d .
O3 O 0.3105(9) 0.1463(8) 0.2272(7) 0.042 Uani 1 1 d .
O4 O 0.336(2) 0.411(2) 0.4222(12) 0.148 Uani 1 1 d .
O5 O 0.539(2) 0.378(2) 0.363(2) 0.147 Uani 1 1 d U
O6 O 0.1527(10) 0.3797(13) 0.2344(10) 0.072 Uani 1 1 d .
O7 O 0.5563(9) 0.3400(9) 0.1197(8) 0.045 Uani 1 1 d .
O8 O 0.7344(10) 0.6521(10) 0.3625(11) 0.060 Uani 1 1 d .
O9 O 0.3217(13) 0.6917(11) 0.4694(10) 0.070 Uani 1 1 d .
O10 O 0.0164(8) 0.5407(9) 0.1037(8) 0.040 Uani 1 1 d .
O11 O 0.0226(7) 0.1394(8) 0.5360(9) 0.042 Uani 1 1 d .
O12 O -0.0539(9) 0.3190(10) 0.4013(8) 0.047 Uani 1 1 d .
H12 H -0.0465 0.2605 0.3486 0.070 Uiso 1 1 calc R
O13 O 0.806(5) 0.474(4) 0.237(5) 0.322 Uani 1 1 d DU
H13 H 0.7409 0.4523 0.1900 0.483 Uiso 1 1 calc R
N1 N 0.5533(9) 0.8065(9) 0.3468(8) 0.031 Uani 1 1 d .
N2 N 0.3904(10) 0.5865(9) 0.0859(9) 0.035 Uani 1 1 d .
N3 N 0.3422(9) 0.4579(9) 0.0674(9) 0.031 Uani 1 1 d .
N4 N 0.2581(10) 0.2161(10) 0.0413(9) 0.037 Uani 1 1 d .
C1 C 0.6696(13) 0.9588(11) 0.5189(12) 0.039 Uani 1 1 d .
H1A H 0.7646 0.9875 0.5234 0.047 Uiso 1 1 calc R
H1B H 0.6373 1.0259 0.5647 0.047 Uiso 1 1 calc R
C2 C 0.6143(11) 0.9264(11) 0.3954(12) 0.036 Uani 1 1 d .
C3 C 0.6245(14) 1.0140(12) 0.3328(11) 0.042 Uani 1 1 d .
H3 H 0.6702 1.0962 0.3668 0.051 Uiso 1 1 calc R
C4 C 0.5681(15) 0.9799(13) 0.2223(13) 0.047 Uani 1 1 d .
H4 H 0.5721 1.0397 0.1818 0.056 Uiso 1 1 calc R
C5 C 0.5025(15) 0.8533(12) 0.1670(12) 0.044 Uani 1 1 d .
H5 H 0.4639 0.8266 0.0908 0.053 Uiso 1 1 calc R
C6 C 0.5013(12) 0.7709(11) 0.2392(11) 0.033 Uani 1 1 d .
C7 C 0.4414(12) 0.6351(11) 0.1891(11) 0.036 Uani 1 1 d .
C8 C 0.2777(12) 0.3914(13) -0.0359(12) 0.042 Uani 1 1 d .
H8 H 0.2633 0.4282 -0.0943 0.050 Uiso 1 1 calc R
C9 C 0.2313(12) 0.2584(13) -0.0514(10) 0.038 Uani 1 1 d .
C10 C 0.1593(14) 0.1800(14) -0.1546(11) 0.045 Uani 1 1 d .
H10 H 0.1368 0.2114 -0.2146 0.054 Uiso 1 1 calc R
C11 C 0.1220(14) 0.0518(13) -0.1639(12) 0.048 Uani 1 1 d .
H11 H 0.0781 -0.0032 -0.2328 0.057 Uiso 1 1 calc R
C12 C 0.1501(13) 0.0070(14) -0.0719(12) 0.047 Uani 1 1 d .
C13 C 0.2167(13) 0.0908(13) 0.0278(12) 0.040 Uani 1 1 d .
C14 C 0.1170(15) -0.1218(13) -0.0742(13) 0.053 Uani 1 1 d .
H14 H 0.0727 -0.1815 -0.1405 0.063 Uiso 1 1 calc R
C15 C 0.1497(15) -0.1558(14) 0.0185(14) 0.055 Uani 1 1 d .
H15 H 0.1314 -0.2400 0.0139 0.066 Uiso 1 1 calc R
C16 C 0.2121(15) -0.0684(12) 0.1254(12) 0.047 Uani 1 1 d .
H16 H 0.2271 -0.0961 0.1901 0.057 Uiso 1 1 calc R
C17 C 0.2499(12) 0.0572(12) 0.1323(11) 0.037 Uani 1 1 d .
C18 C 0.7992(8) 0.3847(9) 0.3003(7) 0.015 Uani 1 1 d D
H18A H 0.8713 0.4134 0.3600 0.022 Uiso 1 1 calc R
H18B H 0.8039 0.3075 0.2489 0.022 Uiso 1 1 calc R
H18C H 0.7178 0.3727 0.3354 0.022 Uiso 1 1 calc R
C19 C 0.073(3) 0.387(3) 0.459(2) 0.116 Uani 1 1 d .
H19A H 0.0889 0.4724 0.4580 0.174 Uiso 1 1 calc R
H19B H 0.1389 0.3526 0.4204 0.174 Uiso 1 1 calc R
H19C H 0.0763 0.3825 0.5385 0.174 Uiso 1 1 calc R
H1H H 0.666(15) 0.857(17) 0.634(6) 0.071 Uiso 1 1 d D
O14 O 0.1695(14) 0.7323(13) 0.3072(13) 0.084 Uani 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'
Dy Dy -0.1892 4.4098 '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
O5 Dy1 O4 62.1(7) . .
O5 Dy1 O3 86.9(6) . .
O4 Dy1 O3 91.2(6) . .
O5 Dy1 O6 136.2(6) . .
O4 Dy1 O6 74.2(6) . .
O3 Dy1 O6 96.4(4) . .
O5 Dy1 O2 83.0(6) . .
O4 Dy1 O2 79.5(6) . .
O3 Dy1 O2 168.6(3) . .
O6 Dy1 O2 87.4(4) . .
O5 Dy1 O7 74.1(6) . .
O4 Dy1 O7 135.4(6) . .
O3 Dy1 O7 94.9(3) . .
O6 Dy1 O7 148.0(4) . .
O2 Dy1 O7 87.3(3) . .
O5 Dy1 N4 141.2(6) . .
O4 Dy1 N4 141.7(7) . .
O3 Dy1 N4 67.0(3) . .
O6 Dy1 N4 77.3(4) . .
O2 Dy1 N4 124.3(3) . .
O7 Dy1 N4 79.8(3) . .
O5 Dy1 N3 132.9(6) . .
O4 Dy1 N3 129.9(4) . .
O3 Dy1 N3 130.6(3) . .
O6 Dy1 N3 74.8(4) . .
O2 Dy1 N3 60.8(3) . .
O7 Dy1 N3 75.2(3) . .
N4 Dy1 N3 63.6(3) . .
O5 Dy1 Dy2 53.8(6) . .
O4 Dy1 Dy2 49.9(7) . .
O3 Dy1 Dy2 132.8(2) . .
O6 Dy1 Dy2 96.5(3) . .
O2 Dy1 Dy2 35.88(19) . .
O7 Dy1 Dy2 97.5(2) . .
N4 Dy1 Dy2 160.2(2) . .
N3 Dy1 Dy2 96.6(2) . .
O5 Dy1 Dy2 34.0(6) . 2_666
O4 Dy1 Dy2 33.1(3) . 2_666
O3 Dy1 Dy2 75.5(2) . 2_666
O6 Dy1 Dy2 104.8(3) . 2_666
O2 Dy1 Dy2 93.12(19) . 2_666
O7 Dy1 Dy2 107.0(2) . 2_666
N4 Dy1 Dy2 142.5(2) . 2_666
N3 Dy1 Dy2 153.8(2) . 2_666
Dy2 Dy1 Dy2 57.23(3) . 2_666
O4 Dy2 O5 62.6(7) 2_666 2_666
O4 Dy2 O2 134.5(5) 2_666 .
O5 Dy2 O2 135.8(6) 2_666 .
O4 Dy2 O1 87.4(7) 2_666 .
O5 Dy2 O1 85.6(6) 2_666 .
O2 Dy2 O1 128.0(3) . .
O4 Dy2 O9 137.0(5) 2_666 .
O5 Dy2 O9 74.4(6) 2_666 .
O2 Dy2 O9 77.5(3) . .
O1 Dy2 O9 90.1(4) . .
O4 Dy2 O8 75.7(5) 2_666 .
O5 Dy2 O8 138.0(6) 2_666 .
O2 Dy2 O8 78.6(3) . .
O1 Dy2 O8 86.9(4) . .
O9 Dy2 O8 146.9(4) . .
O4 Dy2 N1 137.9(7) 2_666 .
O5 Dy2 N1 138.0(6) 2_666 .
O2 Dy2 N1 63.5(3) . .
O1 Dy2 N1 64.5(3) . .
O9 Dy2 N1 76.8(3) . .
O8 Dy2 N1 72.3(3) . .
O4 Dy2 O4 91.4(8) 2_666 .
O5 Dy2 O4 70.9(6) 2_666 .
O2 Dy2 O4 68.7(3) . .
O1 Dy2 O4 154.0(4) . .
O9 Dy2 O4 73.3(4) . .
O8 Dy2 O4 117.9(4) . .
N1 Dy2 O4 127.7(4) . .
O4 Dy2 Dy2 53.0(7) 2_666 2_666
O5 Dy2 Dy2 56.9(6) 2_666 2_666
O2 Dy2 Dy2 98.3(2) . 2_666
O1 Dy2 Dy2 133.7(2) . 2_666
O9 Dy2 Dy2 103.0(3) . 2_666
O8 Dy2 Dy2 102.8(2) . 2_666
N1 Dy2 Dy2 161.6(2) . 2_666
O4 Dy2 Dy2 38.4(3) . 2_666
O4 Dy2 Dy1 104.9(6) 2_666 .
O5 Dy2 Dy1 107.9(6) 2_666 .
O2 Dy2 Dy1 36.8(2) . .
O1 Dy2 Dy1 164.8(2) . .
O9 Dy2 Dy1 86.9(3) . .
O8 Dy2 Dy1 87.5(3) . .
N1 Dy2 Dy1 100.3(2) . .
O4 Dy2 Dy1 37.2(3) . .
Dy2 Dy2 Dy1 61.49(3) 2_666 .
O4 Dy2 Dy1 33.7(3) 2_666 2_666
O5 Dy2 Dy1 34.0(5) 2_666 2_666
O2 Dy2 Dy1 159.6(2) . 2_666
O1 Dy2 Dy1 72.4(2) . 2_666
O9 Dy2 Dy1 105.6(3) . 2_666
O8 Dy2 Dy1 104.8(3) . 2_666
N1 Dy2 Dy1 136.9(2) . 2_666
O4 Dy2 Dy1 92.6(3) . 2_666
Dy2 Dy2 Dy1 61.28(2) 2_666 2_666
Dy1 Dy2 Dy1 122.77(3) . 2_666
C1 O1 Dy2 126.5(8) . .
C7 O2 Dy2 129.2(7) . .
C7 O2 Dy1 123.5(7) . .
Dy2 O2 Dy1 107.3(3) . .
C17 O3 Dy1 121.8(8) . .
Dy2 O4 Dy1 113.2(6) 2_666 .
Dy2 O4 Dy2 88.6(8) 2_666 .
Dy1 O4 Dy2 92.9(7) . .
Dy1 O5 Dy2 112.0(9) . 2_666
C6 N1 C2 119.9(11) . .
C6 N1 Dy2 119.1(8) . .
C2 N1 Dy2 120.9(8) . .
C7 N2 N3 109.8(10) . .
C8 N3 N2 118.2(10) . .
C8 N3 Dy1 120.6(8) . .
N2 N3 Dy1 121.2(7) . .
C9 N4 C13 117.1(11) . .
C9 N4 Dy1 123.4(8) . .
C13 N4 Dy1 119.5(8) . .
O1 C1 C2 111.2(10) . .
N1 C2 C3 121.1(12) . .
N1 C2 C1 116.3(11) . .
C3 C2 C1 122.6(11) . .
C4 C3 C2 120.0(12) . .
C3 C4 C5 120.7(12) . .
C4 C5 C6 114.2(12) . .
N1 C6 C5 124.0(12) . .
N1 C6 C7 116.9(11) . .
C5 C6 C7 119.1(12) . .
N2 C7 O2 124.7(11) . .
N2 C7 C6 124.2(12) . .
O2 C7 C6 111.1(10) . .
N3 C8 C9 116.1(10) . .
N4 C9 C10 122.6(12) . .
N4 C9 C8 116.3(11) . .
C10 C9 C8 121.1(12) . .
C9 C10 C11 117.4(12) . .
C12 C11 C10 120.7(12) . .
C13 C12 C11 118.1(13) . .
C13 C12 C14 117.4(13) . .
C11 C12 C14 124.5(13) . .
N4 C13 C12 124.0(12) . .
N4 C13 C17 112.0(12) . .
C12 C13 C17 124.0(12) . .
C15 C14 C12 120.0(13) . .
C14 C15 C16 122.9(14) . .
C17 C16 C15 120.0(13) . .
O3 C17 C16 124.8(12) . .
O3 C17 C13 119.6(11) . .
C16 C17 C13 115.6(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O5 2.29(2) .
Dy1 O4 2.293(13) .
Dy1 O3 2.306(9) .
Dy1 O6 2.371(11) .
Dy1 O2 2.381(8) .
Dy1 O7 2.416(10) .
Dy1 N4 2.455(10) .
Dy1 N3 2.562(10) .
Dy1 Dy2 3.7919(14) .
Dy1 Dy2 3.7993(17) 2_666
Dy2 O4 2.258(14) 2_666
Dy2 O5 2.29(2) 2_666
Dy2 O2 2.328(8) .
Dy2 O1 2.352(9) .
Dy2 O9 2.400(14) .
Dy2 O8 2.468(12) .
Dy2 N1 2.537(10) .
Dy2 O4 2.91(3) .
Dy2 Dy2 3.6357(18) 2_666
Dy2 Dy1 3.7993(17) 2_666
O1 C1 1.438(15) .
O2 C7 1.337(15) .
O3 C17 1.341(15) .
O4 Dy2 2.258(14) 2_666
O5 Dy2 2.29(2) 2_666
O12 C19 1.43(3) .
O13 C18 1.411(19) .
N1 C6 1.305(16) .
N1 C2 1.342(16) .
N2 C7 1.259(16) .
N2 N3 1.402(14) .
N3 C8 1.339(17) .
N4 C9 1.365(16) .
N4 C13 1.369(17) .
C1 C2 1.491(19) .
C2 C3 1.386(18) .
C3 C4 1.35(2) .
C4 C5 1.428(19) .
C5 C6 1.433(17) .
C6 C7 1.493(17) .
C8 C9 1.453(19) .
C9 C10 1.400(18) .
C10 C11 1.41(2) .
C11 C12 1.38(2) .
C12 C13 1.373(19) .
C12 C14 1.43(2) .
C13 C17 1.454(18) .
C14 C15 1.33(2) .
C15 C16 1.43(2) .
C16 C17 1.385(18) .
