#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:17:09 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143498 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/52/7035252.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_7035252
loop_
_publ_author_name
'Bag, Partha Pratim'
'Wang, Xu-Sheng'
'Cao, Rong'
_publ_section_title
;
 Microwave-assisted large scale synthesis of lanthanide metal-organic
 frameworks (Ln-MOFs), having a preferred conformation and
 photoluminescence properties.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11954
_journal_page_last               11962
_journal_paper_doi               10.1039/c5dt01598g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C30 H27 Cl Dy N5 O14'
_chemical_formula_weight         879.52
_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
_audit_update_record
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                106.106(3)
_cell_angle_beta                 98.088(2)
_cell_angle_gamma                100.255(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4727(2)
_cell_length_b                   12.6520(4)
_cell_length_c                   18.6017(6)
_cell_measurement_reflns_used    10279
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.5230
_cell_measurement_theta_min      4.8270
_cell_volume                     2064.63(11)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15375
_diffrn_reflns_theta_full        73.81
_diffrn_reflns_theta_max         73.81
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    10.828
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.0903
_exptl_crystal_size_mid          0.0611
_exptl_crystal_size_min          0.0407
_platon_squeeze_details
;
;
_refine_diff_density_max         2.904
_refine_diff_density_min         -4.636
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         8016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0714
_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)+(0.1499P)²+4.0441P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.1965
_reflns_number_gt                7584
_reflns_number_total             8016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01598g2.cif
_cod_data_source_block           dy_final
_cod_depositor_comments
'Adding full bibliography for 7035246--7035254.cif.'
_cod_original_cell_volume        2064.63(10)
_cod_database_code               7035252
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 0.76384(3) -0.51563(2) 0.497148(14) 0.01110(15) Uani 1 1 d .
O6 O 1.5516(4) 0.4682(4) 1.4147(2) 0.0190(8) Uani 1 1 d .
N2 N 0.9956(6) 0.3485(4) 0.8172(3) 0.0172(10) Uani 1 1 d .
O1 O 0.9757(4) -0.3919(3) 0.5743(2) 0.0209(9) Uani 1 1 d .
O4 O 0.8895(4) 0.3830(4) 0.5597(2) 0.0215(9) Uani 1 1 d .
O5 O 1.3196(5) 0.4791(4) 1.3867(2) 0.0245(10) Uani 1 1 d .
O2 O 1.2185(5) -0.3323(4) 0.6077(2) 0.0230(9) Uani 1 1 d .
N3 N 1.4388(6) 0.3372(5) 1.1332(3) 0.0227(11) Uani 1 1 d .
C8 C 1.0987(7) 0.0819(5) 0.9264(3) 0.0192(11) Uani 1 1 d .
C27 C 1.4398(6) 0.4201(5) 1.2851(3) 0.0150(10) Uani 1 1 d .
O8 O 0.5887(5) -0.6891(4) 0.4909(3) 0.0318(11) Uani 1 1 d .
N1 N 1.0439(6) -0.1079(4) 0.8262(3) 0.0210(10) Uani 1 1 d .
C10 C 1.0804(6) 0.2684(5) 0.9213(3) 0.0161(11) Uani 1 1 d .
C1 C 1.0905(7) -0.3293(5) 0.6175(4) 0.0214(12) Uani 1 1 d .
C30 C 1.4391(6) 0.4609(5) 1.3706(3) 0.0160(11) Uani 1 1 d .
C28 C 1.5658(6) 0.3981(6) 1.2604(3) 0.0219(12) Uani 1 1 d .
H28 H 1.6538 0.4107 1.2963 0.026 Uiso 1 1 calc R
C2 C 1.0752(7) -0.2439(5) 0.6895(4) 0.0224(12) Uani 1 1 d .
C11 C 1.2187(7) 0.3156(6) 0.9707(3) 0.0244(13) Uani 1 1 d .
C13 C 1.2329(8) 0.1279(6) 0.9771(3) 0.0263(14) Uani 1 1 d .
C26 C 1.3142(6) 0.4021(5) 1.2312(3) 0.0197(11) Uani 1 1 d .
H26 H 1.2277 0.4194 1.2472 0.024 Uiso 1 1 calc R
C12 C 1.2953(11) 0.2455(9) 0.9975(5) 0.0491(9) Uani 1 1 d .
C29 C 1.5625(7) 0.3579(6) 1.1835(4) 0.0258(13) Uani 1 1 d .
H29 H 1.6493 0.3448 1.1661 0.031 Uiso 1 1 calc R
C15 C 0.8781(7) 0.1021(5) 0.8424(4) 0.0262(14) Uani 1 1 d .
H15A H 0.8330 0.1631 0.8346 0.039 Uiso 1 1 calc R
H15B H 0.8128 0.0537 0.8627 0.039 Uiso 1 1 calc R
H15C H 0.8948 0.0571 0.7935 0.039 Uiso 1 1 calc R
C25 C 1.3142(6) 0.3591(6) 1.1540(3) 0.0216(12) Uani 1 1 d .
H25 H 1.2280 0.3454 1.1167 0.026 Uiso 1 1 calc R
C6 C 1.1971(7) -0.1783(5) 0.7445(4) 0.0242(13) Uani 1 1 d .
H6 H 1.2927 -0.1806 0.7352 0.029 Uiso 1 1 calc R
C21 C 0.8754(7) 0.3704(7) 0.7046(4) 0.0312(15) Uani 1 1 d .
H21 H 0.7886 0.3743 0.6739 0.037 Uiso 1 1 calc R
C3 C 0.9370(7) -0.2371(5) 0.7043(4) 0.0246(13) Uani 1 1 d .
H3 H 0.8518 -0.2798 0.6671 0.030 Uiso 1 1 calc R
C19 C 1.1304(7) 0.3677(6) 0.7233(4) 0.0230(12) Uani 1 1 d .
H19 H 1.2201 0.3710 0.7057 0.028 Uiso 1 1 calc R
C4 C 0.9251(7) -0.1682(5) 0.7727(4) 0.0250(13) Uani 1 1 d .
H4 H 0.8307 -0.1629 0.7829 0.030 Uiso 1 1 calc R
C23 C 1.0116(7) 0.3992(5) 0.6024(3) 0.0206(12) Uani 1 1 d .
C9 C 1.0216(6) 0.1518(5) 0.8980(3) 0.0155(10) Uani 1 1 d .
C18 C 1.1222(7) 0.3531(5) 0.7930(4) 0.0219(12) Uani 1 1 d .
H18 H 1.2065 0.3462 0.8241 0.026 Uiso 1 1 calc R
C17 C 0.9916(7) 0.3450(5) 0.8984(3) 0.0216(12) Uani 1 1 d .
H17A H 1.0292 0.4224 0.9345 0.026 Uiso 1 1 calc R
H17B H 0.8887 0.3191 0.9021 0.026 Uiso 1 1 calc R
C16 C 1.2795(10) 0.4416(7) 0.9950(5) 0.046(2) Uani 1 1 d .
H16A H 1.2229 0.4799 1.0300 0.069 Uiso 1 1 calc R
H16B H 1.2729 0.4675 0.9499 0.069 Uiso 1 1 calc R
H16C H 1.3822 0.4592 1.0210 0.069 Uiso 1 1 calc R
C5 C 1.1790(7) -0.1105(5) 0.8121(4) 0.0255(13) Uani 1 1 d .
H5 H 1.2624 -0.0647 0.8495 0.031 Uiso 1 1 calc R
C22 C 0.8733(7) 0.3573(6) 0.7757(4) 0.0275(14) Uani 1 1 d .
H22 H 0.7856 0.3546 0.7951 0.033 Uiso 1 1 calc R
C20 C 1.0058(6) 0.3778(5) 0.6785(3) 0.0197(12) Uani 1 1 d .
C7 C 1.0270(8) -0.0422(5) 0.9038(4) 0.0258(13) Uani 1 1 d .
H7A H 1.0703 -0.0746 0.9420 0.031 Uiso 1 1 calc R
H7B H 0.9214 -0.0507 0.9046 0.031 Uiso 1 1 calc R
C24 C 1.4467(10) 0.2969(9) 1.0492(5) 0.0491(9) Uani 1 1 d .
H24A H 1.5068 0.2397 1.0413 0.059 Uiso 1 1 calc R
H24B H 1.4957 0.3615 1.0346 0.059 Uiso 1 1 calc R
C14 C 1.3194(10) 0.0547(8) 1.0102(4) 0.0415(19) Uani 1 1 d .
H14A H 1.2557 -0.0198 1.0012 0.062 Uiso 1 1 calc R
H14B H 1.3548 0.0913 1.0653 0.062 Uiso 1 1 calc R
H14C H 1.4030 0.0458 0.9853 0.062 Uiso 1 1 calc R
O3 O 1.1361(5) 0.4353(4) 0.5912(3) 0.0235(9) Uani 1 1 d .
O7 O 0.7148(6) -0.3297(4) 0.5236(3) 0.0376(13) Uani 1 1 d .
O9 O 0.4055(6) 0.1316(5) 0.2122(3) 0.0399(13) Uani 1 1 d .
N5 N 0.1003(9) 0.6648(8) 0.9010(4) 0.0491(9) Uani 1 1 d .
N4 N 0.4260(9) 0.1291(7) 0.2788(5) 0.053(2) Uani 1 1 d .
O11 O 0.3883(10) 0.1911(10) 0.3313(4) 0.086(3) Uani 1 1 d .
O10 O 0.4903(11) 0.0516(9) 0.2887(7) 0.094(3) Uani 1 1 d .
O13 O 0.0162(7) 0.6121(6) 0.9278(3) 0.0491(9) Uani 1 1 d .
O12 O 0.0428(17) 0.6513(17) 0.8430(13) 0.270(16) Uani 1 1 d .
Cl1 Cl 0.5006(3) 0.6444(4) 0.1774(2) 0.0967(13) Uani 1 1 d .
O14 O 0.2145(9) 0.7570(9) 0.9310(5) 0.076(2) 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 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O6 Dy1 O1 144.83(16) 1_444 .
O6 Dy1 O4 142.53(16) 1_444 1_545
O1 Dy1 O4 72.55(15) . 1_545
O6 Dy1 O5 99.83(14) 1_444 2_757
O1 Dy1 O5 82.41(16) . 2_757
O4 Dy1 O5 78.56(16) 1_545 2_757
O6 Dy1 O3 80.65(15) 1_444 2_756
O1 Dy1 O3 78.61(16) . 2_756
O4 Dy1 O3 121.40(15) 1_545 2_756
O5 Dy1 O3 145.72(18) 2_757 2_756
O6 Dy1 O2 80.27(15) 1_444 2_746
O1 Dy1 O2 119.41(15) . 2_746
O4 Dy1 O2 78.83(16) 1_545 2_746
O5 Dy1 O2 141.42(17) 2_757 2_746
O3 Dy1 O2 72.76(16) 2_756 2_746
O6 Dy1 O7 73.26(16) 1_444 .
O1 Dy1 O7 73.85(16) . .
O4 Dy1 O7 138.51(17) 1_545 .
O5 Dy1 O7 73.5(2) 2_757 .
O3 Dy1 O7 73.90(19) 2_756 .
O2 Dy1 O7 140.12(18) 2_746 .
O6 Dy1 O8 71.59(16) 1_444 .
O1 Dy1 O8 140.23(16) . .
O4 Dy1 O8 72.23(15) 1_545 .
O5 Dy1 O8 73.06(18) 2_757 .
O3 Dy1 O8 136.80(17) 2_756 .
O2 Dy1 O8 70.45(17) 2_746 .
O7 Dy1 O8 125.51(19) . .
C30 O6 Dy1 179.2(4) . 1_666
C18 N2 C22 122.6(5) . .
C18 N2 C17 119.5(5) . .
C22 N2 C17 117.6(5) . .
C1 O1 Dy1 176.9(4) . .
C23 O4 Dy1 137.5(4) . 1_565
C30 O5 Dy1 131.9(4) . 2_757
C1 O2 Dy1 115.1(4) . 2_746
C29 N3 C25 122.5(5) . .
C29 N3 C24 116.8(6) . .
C25 N3 C24 120.4(6) . .
C13 C8 C9 120.4(6) . .
C13 C8 C7 121.7(6) . .
C9 C8 C7 117.8(5) . .
C26 C27 C28 118.8(5) . .
C26 C27 C30 120.8(5) . .
C28 C27 C30 120.4(5) . .
C4 N1 C5 120.4(5) . .
C4 N1 C7 120.0(5) . .
C5 N1 C7 119.5(6) . .
C9 C10 C11 120.6(6) . .
C9 C10 C17 119.8(5) . .
C11 C10 C17 119.4(5) . .
O1 C1 O2 125.9(6) . .
O1 C1 C2 117.2(6) . .
O2 C1 C2 116.9(5) . .
O6 C30 O5 127.7(5) . .
O6 C30 C27 117.1(5) . .
O5 C30 C27 115.2(5) . .
C29 C28 C27 119.3(6) . .
C6 C2 C3 118.8(6) . .
C6 C2 C1 121.2(6) . .
C3 C2 C1 119.8(5) . .
C12 C11 C10 119.5(7) . .
C12 C11 C16 121.0(8) . .
C10 C11 C16 119.5(7) . .
C8 C13 C12 119.7(6) . .
C8 C13 C14 122.0(7) . .
C12 C13 C14 118.3(7) . .
C27 C26 C25 120.2(6) . .
C11 C12 C13 120.2(8) . .
C11 C12 C24 119.1(9) . .
C13 C12 C24 120.7(8) . .
N3 C29 C28 120.5(6) . .
N3 C25 C26 118.5(5) . .
C5 C6 C2 119.7(6) . .
C22 C21 C20 119.2(6) . .
C4 C3 C2 119.1(6) . .
C18 C19 C20 119.2(6) . .
N1 C4 C3 121.4(6) . .
O3 C23 O4 128.0(5) . .
O3 C23 C20 116.5(5) . .
O4 C23 C20 115.4(5) . .
C10 C9 C8 119.5(5) . .
C10 C9 C15 120.0(5) . .
C8 C9 C15 120.5(5) . .
N2 C18 C19 120.0(6) . .
C10 C17 N2 112.8(5) . .
N1 C5 C6 120.5(6) . .
N2 C22 C21 119.6(6) . .
C21 C20 C19 119.4(5) . .
C21 C20 C23 119.6(5) . .
C19 C20 C23 121.0(5) . .
N1 C7 C8 113.3(5) . .
N3 C24 C12 112.3(7) . .
C23 O3 Dy1 137.5(4) . 2_756
O12 N5 O13 105.0(12) . .
O12 N5 O14 116.4(10) . .
O13 N5 O14 134.2(8) . .
O11 N4 O9 125.1(9) . .
O11 N4 O10 121.0(10) . .
O9 N4 O10 113.8(9) . .
N5 O13 O12 35.4(5) . .
N5 O12 O13 39.5(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O6 2.290(4) 1_444
Dy1 O1 2.316(4) .
Dy1 O4 2.324(4) 1_545
Dy1 O5 2.358(4) 2_757
Dy1 O3 2.378(4) 2_756
Dy1 O2 2.379(4) 2_746
Dy1 O7 2.408(5) .
Dy1 O8 2.468(5) .
O6 C30 1.223(7) .
O6 Dy1 2.290(4) 1_666
N2 C18 1.336(8) .
N2 C22 1.339(8) .
N2 C17 1.528(7) .
O1 C1 1.245(7) .
O4 C23 1.255(7) .
O4 Dy1 2.324(4) 1_565
O5 C30 1.254(7) .
O5 Dy1 2.358(4) 2_757
O2 C1 1.257(8) .
O2 Dy1 2.379(4) 2_746
N3 C29 1.327(8) .
N3 C25 1.344(8) .
N3 C24 1.521(9) .
C8 C13 1.392(9) .
C8 C9 1.406(8) .
C8 C7 1.509(8) .
C27 C26 1.383(8) .
C27 C28 1.384(8) .
C27 C30 1.531(7) .
N1 C4 1.340(9) .
N1 C5 1.347(9) .
N1 C7 1.498(8) .
C10 C9 1.400(8) .
C10 C11 1.412(8) .
C10 C17 1.499(8) .
C1 C2 1.513(9) .
C28 C29 1.373(9) .
C2 C6 1.387(9) .
C2 C3 1.388(9) .
C11 C12 1.390(12) .
C11 C16 1.509(10) .
C13 C12 1.421(13) .
C13 C14 1.534(9) .
C26 C25 1.388(8) .
C12 C24 1.529(14) .
C15 C9 1.500(8) .
C6 C5 1.364(9) .
C21 C22 1.381(9) .
C21 C20 1.386(9) .
C3 C4 1.361(9) .
C19 C18 1.370(9) .
C19 C20 1.392(8) .
C23 O3 1.254(7) .
C23 C20 1.521(8) .
O3 Dy1 2.378(4) 2_756
O9 N4 1.237(11) .
N5 O12 1.091(17) .
N5 O13 1.198(10) .
N5 O14 1.364(13) .
N4 O11 1.213(12) .
N4 O10 1.284(12) .
O13 O12 1.82(2) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.010 0.000 0.500 562.4 155.0
