#------------------------------------------------------------------------------
#$Date: 2019-11-23 14:00:49 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233539 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/90/4349008.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_4349008
loop_
_publ_author_name
'Mukherjee, Soumya'
'Lu, Jingjing'
'Velmurugan, Gunasekaran'
'Singh, Shweta'
'Rajaraman, Gopalan'
'Tang, Jinkui'
'Ghosh, Sujit K.'
_publ_section_title
;
 Influence of Tuned Linker Functionality on Modulation of Magnetic
 Properties and Relaxation Dynamics in a Family of Six Isotypic
 Ln₂ (Ln = Dy and Gd) Complexes.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11283
_journal_page_last               11298
_journal_paper_doi               10.1021/acs.inorgchem.6b01863
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C46 H48 Dy2 N2 O14'
_chemical_formula_sum            'C46 H48 Dy2 N2 O14'
_chemical_formula_weight         1177.85
_chemical_name_common            Compound3a
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5275(15)
_cell_length_b                   20.048(3)
_cell_length_c                   25.023(4)
_cell_measurement_reflns_used    8755
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.42
_cell_volume                     4277.9(12)
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27474
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.628
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.539
_exptl_absorpt_correction_T_max  0.7654
_exptl_absorpt_correction_T_min  0.7045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan absorption'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       rod
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.977
_refine_diff_density_min         -2.149
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       0.00013(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4343
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0439P)²+43.2951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2994
_reflns_number_total             4343
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01863_si_006.cif
_cod_data_source_block           Compound3a
_cod_database_code               4349008
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Dy01 Dy 0.51942(5) 0.04111(2) 0.06892(2) 0.02134(16) Uani 1 1 d . U
O2 O 0.7332(8) 0.2452(3) 0.1246(2) 0.0349(16) Uani 1 1 d . U
O1 O 0.6027(7) 0.1265(3) 0.1161(2) 0.0261(13) Uani 1 1 d . U
O5 O 0.7942(8) 0.0069(3) 0.0911(2) 0.0267(13) Uani 1 1 d . U
O3 O 0.4754(7) -0.0697(3) 0.0909(2) 0.0253(13) Uani 1 1 d . U
O7 O 0.7493(7) -0.0975(3) -0.0738(2) 0.0274(13) Uani 1 1 d . U
O6 O 0.6498(7) -0.0130(2) -0.0003(2) 0.0206(12) Uani 1 1 d . U
O4 O 0.5426(7) 0.1278(3) 0.0030(2) 0.0269(14) Uani 1 1 d . U
N1 N 0.4257(9) 0.0252(3) 0.1634(3) 0.0234(15) Uani 1 1 d . U
C21 C 0.8416(10) -0.0909(4) -0.0291(3) 0.0216(17) Uani 1 1 d . U
C10 C 0.2279(10) -0.0482(4) 0.2087(3) 0.0272(18) Uani 1 1 d . U
H4 H 0.2038 -0.0155 0.2337 0.033 Uiso 1 1 calc R U
C22 C 0.7828(10) -0.0466(4) 0.0086(3) 0.0207(16) Uani 1 1 d . U
C14 C 0.3767(11) -0.0837(4) 0.1300(3) 0.0237(18) Uani 1 1 d . U
C1 C 0.5999(11) 0.1555(4) 0.1624(3) 0.0251(19) Uani 1 1 d . U
C7 C 0.5257(10) 0.1256(3) 0.2077(3) 0.0200(17) Uani 1 1 d . U
C4 C 0.6610(11) 0.2517(4) 0.2186(4) 0.030(2) Uani 1 1 d . U
H8 H 0.7051 0.2939 0.2222 0.036 Uiso 1 1 calc R U
C17 C 0.8677(11) -0.0362(4) 0.0561(3) 0.0234(17) Uani 1 1 d . U
C2 C 0.6650(11) 0.2196(4) 0.1699(3) 0.0270(19) Uani 1 1 d . U
C9 C 0.3425(11) -0.0352(4) 0.1694(3) 0.0249(18) Uani 1 1 d . U
C15 C 0.8665(13) 0.0170(5) 0.1410(4) 0.037(2) Uani 1 1 d . U
H9 H 0.8753 -0.0249 0.1594 0.055 Uiso 1 1 calc R U
H14 H 0.8044 0.0472 0.1620 0.055 Uiso 1 1 calc R U
H10 H 0.9691 0.0356 0.1358 0.055 Uiso 1 1 calc R U
C16 C 0.5313(13) 0.1993(4) 0.0065(4) 0.035(2) Uani 1 1 d . U
H17 H 0.4356 0.2138 -0.0100 0.053 Uiso 1 1 calc R U
H16 H 0.6189 0.2192 -0.0115 0.053 Uiso 1 1 calc R U
H15 H 0.5319 0.2125 0.0434 0.053 Uiso 1 1 calc R U
C18 C 1.0055(11) -0.0693(4) 0.0652(4) 0.0295(19) Uani 1 1 d . U
H18 H 1.0596 -0.0631 0.0971 0.035 Uiso 1 1 calc R U
C19 C 1.0636(11) -0.1121(4) 0.0264(4) 0.028(2) Uani 1 1 d . U
H19 H 1.1586 -0.1337 0.0322 0.034 Uiso 1 1 calc R U
C8 C 0.4503(11) 0.0621(4) 0.2053(3) 0.0259(19) Uani 1 1 d . U
H5 H 0.4143 0.0450 0.2376 0.031 Uiso 1 1 calc R U
C20 C 0.9841(11) -0.1235(4) -0.0204(3) 0.0258(18) Uani 1 1 d . U
H20 H 1.0246 -0.1524 -0.0459 0.031 Uiso 1 1 calc R U
C3 C 0.7776(13) 0.3137(4) 0.1265(4) 0.038(2) Uani 1 1 d . U
H11 H 0.6943 0.3394 0.1421 0.058 Uiso 1 1 calc R U
H13 H 0.7975 0.3295 0.0909 0.058 Uiso 1 1 calc R U
H12 H 0.8707 0.3185 0.1476 0.058 Uiso 1 1 calc R U
C13 C 0.2995(11) -0.1463(4) 0.1344(4) 0.030(2) Uani 1 1 d . U
H1 H 0.3224 -0.1798 0.1099 0.036 Uiso 1 1 calc R U
C12 C 0.1919(12) -0.1583(4) 0.1739(4) 0.035(2) Uani 1 1 d . U
H2 H 0.1452 -0.2001 0.1764 0.042 Uiso 1 1 calc R U
C5 C 0.5905(13) 0.2208(4) 0.2623(4) 0.035(2) Uani 1 1 d . U
H7 H 0.5892 0.2423 0.2953 0.042 Uiso 1 1 calc R U
C6 C 0.5235(13) 0.1595(4) 0.2571(4) 0.035(2) Uani 1 1 d . U
H6 H 0.4756 0.1397 0.2865 0.042 Uiso 1 1 calc R U
C23 C 0.7858(12) -0.1512(4) -0.1093(4) 0.033(2) Uani 1 1 d . U
H22 H 0.8866 -0.1436 -0.1252 0.050 Uiso 1 1 calc R U
H23 H 0.7075 -0.1537 -0.1368 0.050 Uiso 1 1 calc R U
H21 H 0.7877 -0.1924 -0.0897 0.050 Uiso 1 1 calc R U
C11 C 0.1515(11) -0.1084(4) 0.2107(4) 0.033(2) Uani 1 1 d . U
H3 H 0.0739 -0.1159 0.2361 0.040 Uiso 1 1 calc R U
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
O1 Dy01 O6 142.22(19) . 5_655
O1 Dy01 O3 132.19(19) . .
O6 Dy01 O3 80.87(19) 5_655 .
O1 Dy01 O6 127.5(2) . .
O6 Dy01 O6 68.4(2) 5_655 .
O3 Dy01 O6 78.87(19) . .
O1 Dy01 O4 77.2(2) . .
O6 Dy01 O4 73.64(19) 5_655 .
O3 Dy01 O4 150.26(19) . .
O6 Dy01 O4 77.70(18) . .
O1 Dy01 O5 78.0(2) . .
O6 Dy01 O5 132.97(18) 5_655 .
O3 Dy01 O5 80.6(2) . .
O6 Dy01 O5 65.79(19) . .
O4 Dy01 O5 105.8(2) . .
O1 Dy01 N1 72.4(2) . .
O6 Dy01 N1 117.9(2) 5_655 .
O3 Dy01 N1 66.7(2) . .
O6 Dy01 N1 142.39(19) . .
O4 Dy01 N1 139.7(2) . .
O5 Dy01 N1 93.1(2) . .
O1 Dy01 O7 85.4(2) . 5_655
O6 Dy01 O7 65.44(18) 5_655 5_655
O3 Dy01 O7 105.5(2) . 5_655
O6 Dy01 O7 132.04(18) . 5_655
O4 Dy01 O7 77.68(19) . 5_655
O5 Dy01 O7 161.58(18) . 5_655
N1 Dy01 O7 74.1(2) . 5_655
O1 Dy01 Dy01 147.71(14) . 5_655
O6 Dy01 Dy01 34.31(14) 5_655 5_655
O3 Dy01 Dy01 77.72(14) . 5_655
O6 Dy01 Dy01 34.08(14) . 5_655
O4 Dy01 Dy01 72.61(13) . 5_655
O5 Dy01 Dy01 99.34(12) . 5_655
N1 Dy01 Dy01 139.70(15) . 5_655
O7 Dy01 Dy01 98.94(12) 5_655 5_655
C2 O2 C3 116.4(7) . .
C1 O1 Dy01 145.3(5) . .
C17 O5 C15 117.0(7) . .
C17 O5 Dy01 117.1(5) . .
C15 O5 Dy01 124.5(5) . .
C14 O3 Dy01 118.8(5) . .
C21 O7 C23 117.0(7) . .
C21 O7 Dy01 115.6(5) . 5_655
C23 O7 Dy01 123.9(5) . 5_655
C22 O6 Dy01 122.0(5) . 5_655
C22 O6 Dy01 121.1(5) . .
Dy01 O6 Dy01 111.6(2) 5_655 .
C16 O4 Dy01 132.2(5) . .
C8 N1 C9 119.0(7) . .
C8 N1 Dy01 129.4(6) . .
C9 N1 Dy01 111.6(5) . .
O7 C21 C22 114.1(7) . .
O7 C21 C20 125.5(7) . .
C22 C21 C20 120.4(8) . .
C11 C10 C9 121.2(8) . .
O6 C22 C21 121.0(7) . .
O6 C22 C17 120.1(7) . .
C21 C22 C17 118.8(8) . .
O3 C14 C9 120.2(7) . .
O3 C14 C13 122.6(7) . .
C9 C14 C13 117.3(8) . .
O1 C1 C2 121.2(8) . .
O1 C1 C7 122.0(7) . .
C2 C1 C7 116.7(7) . .
C6 C7 C8 117.4(8) . .
C6 C7 C1 119.9(7) . .
C8 C7 C1 122.6(7) . .
C2 C4 C5 119.8(8) . .
C18 C17 O5 126.0(8) . .
C18 C17 C22 120.7(8) . .
O5 C17 C22 113.2(7) . .
O2 C2 C4 124.4(8) . .
O2 C2 C1 113.4(7) . .
C4 C2 C1 122.3(8) . .
N1 C9 C10 125.5(7) . .
N1 C9 C14 114.4(7) . .
C10 C9 C14 120.1(8) . .
C17 C18 C19 119.3(8) . .
C20 C19 C18 121.6(8) . .
N1 C8 C7 127.9(8) . .
C19 C20 C21 119.1(8) . .
C12 C13 C14 121.4(8) . .
C13 C12 C11 120.8(8) . .
C6 C5 C4 120.5(8) . .
C5 C6 C7 120.8(9) . .
C10 C11 C12 119.1(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy01 O1 2.198(5) .
Dy01 O6 2.313(5) 5_655
Dy01 O3 2.319(5) .
Dy01 O6 2.326(5) .
Dy01 O4 2.405(5) .
Dy01 O5 2.503(6) .
Dy01 N1 2.516(7) .
Dy01 O7 2.559(6) 5_655
Dy01 Dy01 3.8370(9) 5_655
O2 C2 1.376(10) .
O2 C3 1.426(10) .
O1 C1 1.296(10) .
O5 C17 1.380(10) .
O5 C15 1.409(10) .
O3 C14 1.323(10) .
O7 C21 1.373(10) .
O7 C23 1.429(9) .
O7 Dy01 2.559(6) 5_655
O6 C22 1.337(10) .
O6 Dy01 2.313(5) 5_655
O4 C16 1.438(9) .
N1 C8 1.300(10) .
N1 C9 1.411(10) .
C21 C22 1.390(11) .
C21 C20 1.397(12) .
C10 C11 1.371(12) .
C10 C9 1.411(12) .
C22 C17 1.408(11) .
C14 C9 1.413(11) .
C14 C13 1.421(11) .
C1 C2 1.412(11) .
C1 C7 1.429(11) .
C7 C6 1.411(11) .
C7 C8 1.428(11) .
C4 C2 1.377(12) .
C4 C5 1.394(13) .
C17 C18 1.368(12) .
C18 C19 1.389(12) .
C19 C20 1.371(12) .
C13 C12 1.370(13) .
C12 C11 1.402(13) .
C5 C6 1.362(12) .
