#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:13:32 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179051 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/13/4301312.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_4301312
loop_
_publ_author_name
'Cory A. Black'
'José Sánchez Costa'
'Wen Tian Fu'
'Chiara Massera'
'Olivier Roubeau'
'Simon J. Teat'
'Guillem Aromí'
'Patrick Gamez'
'Jan Reedijk'
_publ_contact_author             'Reedijk, J.'
_publ_contact_author_email       reedijk@chem.leidenuniv.nl
_publ_section_title
;
3-D Lanthanide Metal-Organic Frameworks: Structure, Photoluminescence, and
Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1062
_journal_page_last               1068
_journal_paper_doi               10.1021/ic8017826
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C42 H57 Dy2 N9 O18'
_chemical_formula_sum            'C42 H57 Dy2 N9 O18'
_chemical_formula_weight         1300.97
_chemical_name_common            'compound 5'
_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                100.9550(10)
_cell_angle_beta                 110.4500(10)
_cell_angle_gamma                99.9390(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5059(9)
_cell_length_b                   11.1476(9)
_cell_length_c                   12.7931(10)
_cell_measurement_reflns_used    10725
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      1.76
_cell_volume                     1330.93(19)
_computing_data_collection       SMART
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'BRUKER AXS SMART 1000'
_diffrn_measurement_method       omega-scan
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17279
_diffrn_reflns_theta_full        29.94
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.861
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.665550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.384
_refine_diff_density_min         -2.091
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         7103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0431
_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)+(0.0689P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                5657
_reflns_number_total             7103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8017826_si_002_1.cif
_cod_data_source_block           5
_cod_database_code               4301312
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.60672(2) 0.049092(19) 0.175851(19) 0.02501(8) Uani 1 1 d . . .
O1 O 0.6582(4) 0.0056(4) 0.0143(4) 0.0383(8) Uani 1 1 d . . .
O2 O 0.6191(4) -0.0584(4) -0.1699(3) 0.0416(9) Uani 1 1 d . . .
O3 O 0.5674(4) 0.2197(3) 0.0966(3) 0.0373(8) Uani 1 1 d . . .
O4 O 0.4992(4) 0.1693(3) -0.0961(3) 0.0389(9) Uani 1 1 d . . .
O5 O 0.8323(4) 0.2070(4) 0.2621(4) 0.0570(12) Uani 1 1 d . . .
O6 O 0.6817(4) 0.2350(4) 0.3405(3) 0.0416(9) Uani 1 1 d . . .
O7 O 0.5824(5) -0.0286(4) 0.3324(4) 0.0517(11) Uani 1 1 d . . .
O8 O 0.7946(5) -0.0474(6) 0.2519(5) 0.0692(15) Uani 1 1 d . . .
C1 C 0.7019(5) -0.0228(5) -0.0651(5) 0.0344(11) Uani 1 1 d . . .
C2 C 0.8557(5) -0.0126(5) -0.0326(5) 0.0353(11) Uani 1 1 d . . .
C3 C 1.0932(6) 0.0577(6) 0.1158(5) 0.0439(14) Uani 1 1 d . . .
C4 C 0.9489(6) 0.0451(6) 0.0815(5) 0.0454(14) Uani 1 1 d . . .
H4 H 0.9144 0.0759 0.1361 0.13(2) Uiso 1 1 calc R . .
C5 C 0.5289(6) 0.2455(4) 0.0020(4) 0.0343(11) Uani 1 1 d . . .
C6 C 0.5161(6) 0.3784(4) 0.0020(5) 0.0395(13) Uani 1 1 d . . .
C7 C 0.5140(8) 0.4593(5) 0.0995(5) 0.0472(15) Uani 1 1 d . . .
C8 C 0.5026(8) 0.4200(5) -0.0953(5) 0.0487(15) Uani 1 1 d . . .
H8 H 0.5045 0.3662 -0.1596 0.13(2) Uiso 1 1 calc R . .
C9 C 0.7993(6) 0.2706(5) 0.3350(5) 0.0365(11) Uani 1 1 d . . .
C10 C 0.9024(6) 0.3898(5) 0.4196(4) 0.0390(12) Uani 1 1 d . . .
C11 C 1.1363(7) 0.5313(6) 0.5048(5) 0.0520(16) Uani 1 1 d . . .
C12 C 1.0386(7) 0.4209(6) 0.4246(6) 0.0547(17) Uani 1 1 d . . .
C13 C 0.4814(11) -0.1069(8) 0.3309(7) 0.075(2) Uani 1 1 d . . .
H13 H 0.3979 -0.1259 0.2658 0.13(2) Uiso 1 1 calc R . .
C14 C 0.605(2) -0.1442(17) 0.5102(13) 0.173(5) Uani 1 1 d . . .
H14A H 0.6526 -0.2083 0.4973 0.260 Uiso 1 1 calc R . .
H14B H 0.5809 -0.1484 0.5753 0.260 Uiso 1 1 calc R . .
H14C H 0.6662 -0.0624 0.5257 0.260 Uiso 1 1 calc R . .
C15 C 0.359(2) -0.2526(16) 0.4020(16) 0.189(7) Uani 1 1 d . . .
H15A H 0.3754 -0.3353 0.3938 0.283 Uiso 1 1 calc R . .
H15B H 0.2777 -0.2541 0.3365 0.283 Uiso 1 1 calc R . .
H15C H 0.3437 -0.2277 0.4717 0.283 Uiso 1 1 calc R . .
C16 C 0.8095(13) -0.1403(12) 0.2602(12) 0.118(4) Uani 1 1 d . . .
H16 H 0.7309 -0.2056 0.2107 0.13(2) Uiso 1 1 calc R . .
C17 C 0.894(2) -0.3162(18) 0.3067(18) 0.208(8) Uani 1 1 d . . .
H17A H 0.8310 -0.3613 0.2285 0.312 Uiso 1 1 calc R . .
H17B H 0.8561 -0.3429 0.3594 0.312 Uiso 1 1 calc R . .
H17C H 0.9840 -0.3336 0.3223 0.312 Uiso 1 1 calc R . .
C18 C 1.035(3) -0.108(3) 0.386(2) 0.315(18) Uani 1 1 d . . .
H18A H 1.0346 -0.0219 0.3856 0.472 Uiso 1 1 calc R . .
H18B H 1.1003 -0.1326 0.3545 0.472 Uiso 1 1 calc R . .
H18C H 1.0619 -0.1154 0.4634 0.472 Uiso 1 1 calc R . .
N1 N 1.1758(12) 0.1163(15) 0.2248(9) 0.072(4) Uani 0.50 1 d P . .
N2 N 0.5206(17) 0.4222(11) 0.2036(11) 0.068(4) Uani 0.50 1 d P . .
N3 N 1.279(2) 0.534(2) 0.5216(19) 0.054(6) Uani 0.25 1 d P . .
N3' N 1.095(3) 0.347(3) 0.357(3) 0.107(14) Uani 0.25 1 d P . .
N4 N 0.4782(12) -0.1646(9) 0.4077(8) 0.113(3) Uani 1 1 d . . .
N5 N 0.9092(13) -0.1814(14) 0.3218(12) 0.139(5) 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
_geom_angle_publ_flag
O1 Dy1 O1 75.66(13) . 2_655 ?
O1 Dy1 O2 124.06(14) . 2_655 ?
O1 Dy1 O3 76.27(13) . . ?
O1 Dy1 O4 77.62(13) . 2_655 ?
O1 Dy1 O5 85.10(15) . . ?
O1 Dy1 O6 133.67(13) . . ?
O1 Dy1 O7 144.86(15) . . ?
O1 Dy1 O8 82.17(18) . . ?
O1 Dy1 C1 100.48(14) . 2_655 ?
O1 Dy1 C1 24.87(13) 2_655 2_655 ?
O1 Dy1 C9 109.42(15) . . ?
O2 Dy1 O1 48.58(12) 2_655 2_655 ?
O2 Dy1 O5 132.09(15) 2_655 . ?
O2 Dy1 O6 82.30(14) 2_655 . ?
O2 Dy1 O7 73.49(16) 2_655 . ?
O2 Dy1 O8 142.51(18) 2_655 . ?
O2 Dy1 C1 23.71(14) 2_655 2_655 ?
O2 Dy1 C9 107.46(16) 2_655 . ?
O3 Dy1 O1 65.81(12) . 2_655 ?
O3 Dy1 O2 77.16(14) . 2_655 ?
O3 Dy1 O5 74.41(16) . . ?
O3 Dy1 O6 73.92(13) . . ?
O3 Dy1 O7 138.70(15) . . ?
O3 Dy1 O8 139.35(18) . . ?
O3 Dy1 C1 70.32(14) . 2_655 ?
O3 Dy1 C9 71.75(14) . . ?
O4 Dy1 O1 67.27(12) 2_655 2_655 ?
O4 Dy1 O2 83.83(14) 2_655 2_655 ?
O4 Dy1 O3 130.43(13) 2_655 . ?
O4 Dy1 O5 143.26(15) 2_655 . ?
O4 Dy1 O6 147.84(13) 2_655 . ?
O4 Dy1 O7 74.38(14) 2_655 . ?
O4 Dy1 O8 75.93(18) 2_655 . ?
O4 Dy1 C1 74.04(14) 2_655 2_655 ?
O4 Dy1 C9 157.59(15) 2_655 . ?
O5 Dy1 O1 138.77(15) . 2_655 ?
O5 Dy1 O6 53.17(14) . . ?
O5 Dy1 C1 141.66(16) . 2_655 ?
O5 Dy1 C9 26.41(16) . . ?
O6 Dy1 O1 120.88(13) . 2_655 ?
O6 Dy1 C1 101.83(14) . 2_655 ?
O6 Dy1 C9 26.77(15) . . ?
O7 Dy1 O1 111.51(14) . 2_655 ?
O7 Dy1 O5 105.24(17) . . ?
O7 Dy1 O6 73.90(14) . . ?
O7 Dy1 O8 70.83(19) . . ?
O7 Dy1 C1 91.84(16) . 2_655 ?
O7 Dy1 C9 90.03(15) . . ?
O8 Dy1 O1 140.14(17) . 2_655 ?
O8 Dy1 O5 69.71(19) . . ?
O8 Dy1 O6 98.39(18) . . ?
O8 Dy1 C1 148.46(18) . 2_655 ?
O8 Dy1 C9 83.86(19) . . ?
C9 Dy1 O1 134.65(13) . 2_655 ?
C9 Dy1 C1 123.41(15) . 2_655 ?
Dy1 O1 Dy1 104.34(13) . 2_655 ?
C1 O1 Dy1 171.6(4) . . ?
C1 O1 Dy1 83.3(3) . 2_655 ?
C1 O2 Dy1 106.9(3) . 2_655 ?
C5 O3 Dy1 141.0(3) . . ?
C5 O4 Dy1 133.3(3) . 2_655 ?
C9 O5 Dy1 93.2(3) . . ?
C9 O6 Dy1 92.4(3) . . ?
C13 O7 Dy1 128.5(5) . . ?
C16 O8 Dy1 139.4(8) . . ?
O1 C1 Dy1 71.9(3) . 2_655 ?
O1 C1 C2 118.9(5) . . ?
O2 C1 Dy1 49.4(2) . 2_655 ?
O2 C1 O1 121.2(5) . . ?
O2 C1 C2 119.9(5) . . ?
C2 C1 Dy1 169.1(4) . 2_655 ?
C3 C2 C1 121.0(5) 2_755 . ?
C4 C2 C1 119.2(5) . . ?
C4 C2 C3 119.8(5) . 2_755 ?
C4 C3 C2 118.9(5) . 2_755 ?
N1 C3 C2 123.0(7) . 2_755 ?
N1 C3 C4 118.0(7) . . ?
C2 C4 H4 119.4 . . ?
C2 C4 C3 121.3(5) . . ?
C3 C4 H4 119.4 . . ?
O3 C5 O4 125.6(4) . . ?
O3 C5 C6 117.8(5) . . ?
O4 C5 C6 116.6(4) . . ?
C7 C6 C5 120.4(5) . . ?
C8 C6 C5 120.1(5) . . ?
C8 C6 C7 119.4(5) . . ?
C6 C7 N2 123.5(6) . . ?
C8 C7 C6 119.0(5) 2_665 . ?
C8 C7 N2 117.4(7) 2_665 . ?
C6 C8 H8 119.2 . . ?
C6 C8 C7 121.5(6) . 2_665 ?
C7 C8 H8 119.2 2_665 . ?
O5 C9 Dy1 60.4(3) . . ?
O5 C9 O6 121.2(5) . . ?
O5 C9 C10 119.5(5) . . ?
O6 C9 Dy1 60.8(3) . . ?
O6 C9 C10 119.3(5) . . ?
C10 C9 Dy1 179.5(4) . . ?
C11 C10 C9 120.6(5) 2_766 . ?
C12 C10 C9 119.8(6) . . ?
C12 C10 C11 119.6(5) . 2_766 ?
C10 C11 C12 120.4(6) 2_766 . ?
C10 C11 N3 123.9(10) 2_766 . ?
C12 C11 N3 113.6(10) . . ?
C10 C12 C11 120.1(6) . . ?
C10 C12 N3' 126.1(11) . . ?
C11 C12 N3' 113.8(11) . . ?
O7 C13 H13 116.0 . . ?
O7 C13 N4 128.0(10) . . ?
N4 C13 H13 116.0 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
O8 C16 H16 112.2 . . ?
O8 C16 N5 135.6(14) . . ?
N5 C16 H16 112.2 . . ?
H17B C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N5 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
N5 C18 H18C 109.5 . . ?
C13 N4 C14 119.7(11) . . ?
C13 N4 C15 125.7(13) . . ?
C15 N4 C14 114.6(11) . . ?
C16 N5 C17 120.6(15) . . ?
C16 N5 C18 122.2(18) . . ?
C18 N5 C17 116.3(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.300(4) . ?
Dy1 O1 2.856(4) 2_655 ?
Dy1 O2 2.368(4) 2_655 ?
Dy1 O3 2.351(3) . ?
Dy1 O4 2.353(3) 2_655 ?
Dy1 O5 2.434(4) . ?
Dy1 O6 2.444(4) . ?
Dy1 O7 2.402(4) . ?
Dy1 O8 2.406(4) . ?
Dy1 C9 2.796(5) . ?
Dy1 C1 2.985(5) 2_655 ?
O1 Dy1 2.856(4) 2_655 ?
O1 C1 1.264(6) . ?
O2 Dy1 2.368(4) 2_655 ?
O2 C1 1.255(7) . ?
O3 C5 1.242(6) . ?
O4 Dy1 2.353(3) 2_655 ?
O4 C5 1.274(6) . ?
O5 C9 1.246(7) . ?
O6 C9 1.261(7) . ?
O7 C13 1.244(9) . ?
O8 C16 1.092(11) . ?
C1 Dy1 2.985(5) 2_655 ?
C1 C2 1.499(7) . ?
C2 C3 1.401(7) 2_755 ?
C2 C4 1.389(8) . ?
C3 C2 1.401(7) 2_755 ?
C3 C4 1.396(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.510(7) . ?
C6 C7 1.403(8) . ?
C6 C8 1.380(8) . ?
C7 C8 1.395(8) 2_665 ?
C8 H8 0.9300 . ?
C8 C7 1.395(8) 2_665 ?
C9 C10 1.500(7) . ?
C10 C11 1.396(9) 2_766 ?
C10 C12 1.389(9) . ?
C11 C10 1.396(9) 2_766 ?
C11 C12 1.403(8) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
N1 C3 1.317(12) . ?
N2 C7 1.451(13) . ?
N3 C11 1.43(2) . ?
N3' C12 1.42(3) . ?
N4 C13 1.279(11) . ?
N4 C14 1.454(19) . ?
N4 C15 1.420(15) . ?
N5 C16 1.285(12) . ?
N5 C17 1.45(2) . ?
N5 C18 1.30(3) . ?
