#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:17:09 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143498 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/52/7035248.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_7035248
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 N5 O14 Pr'
_chemical_formula_weight         857.93
_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                105.932(3)
_cell_angle_beta                 98.860(2)
_cell_angle_gamma                100.482(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5300(3)
_cell_length_b                   12.5401(4)
_cell_length_c                   18.8719(6)
_cell_measurement_reflns_used    8734
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.1470
_cell_measurement_theta_min      4.8020
_cell_volume                     2082.30(12)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15822
_diffrn_reflns_theta_full        73.85
_diffrn_reflns_theta_max         73.85
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    10.111
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.0723
_exptl_crystal_size_mid          0.0451
_exptl_crystal_size_min          0.0273
_platon_squeeze_details
;
;
_refine_diff_density_max         2.582
_refine_diff_density_min         -1.685
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0559
_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)+(0.1196P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                7213
_reflns_number_total             8023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01598g2.cif
_cod_data_source_block           pr_final
_cod_depositor_comments
'Adding full bibliography for 7035246--7035254.cif.'
_cod_original_cell_volume        2082.30(11)
_cod_database_code               7035248
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
Pr1 Pr -0.23418(3) 0.48222(2) 0.496364(12) 0.02345(12) Uani 1 1 d .
O6 O -0.5437(4) -0.4702(4) -0.41333(19) 0.0332(8) Uani 1 1 d .
O5 O -0.3133(4) -0.4802(4) -0.38256(19) 0.0346(9) Uani 1 1 d .
N2 N 0.0035(5) -0.3481(4) 0.1816(3) 0.0266(9) Uani 1 1 d .
N3 N -0.4327(5) -0.3371(5) -0.1337(3) 0.0331(6) Uani 1 1 d .
N1 N -0.0430(5) 0.1100(4) 0.1741(3) 0.0309(10) Uani 1 1 d .
O1 O -0.2332(4) 0.3198(4) 0.3856(2) 0.0397(10) Uani 1 1 d .
C8 C -0.0946(6) -0.0799(5) 0.0733(3) 0.0282(11) Uani 1 1 d .
C9 C -0.0201(5) -0.1508(4) 0.1016(3) 0.0252(10) Uani 1 1 d .
C30 C -0.4319(6) -0.4619(5) -0.3673(3) 0.0263(10) Uani 1 1 d .
O2 O 0.0063(4) 0.3913(3) 0.4249(2) 0.0342(8) Uani 1 1 d .
C10 C -0.0774(6) -0.2681(4) 0.0780(3) 0.0265(10) Uani 1 1 d .
O3 O -0.1388(4) -0.4306(4) 0.4050(2) 0.0394(10) Uani 1 1 d .
C13 C -0.2274(6) -0.1242(5) 0.0225(3) 0.0330(12) Uani 1 1 d .
C2 C -0.0793(6) 0.2434(5) 0.3074(3) 0.0308(11) Uani 1 1 d .
C12 C -0.2898(6) -0.2443(6) 0.0013(3) 0.0345(12) Uani 1 1 d .
C26 C -0.3086(6) -0.4018(5) -0.2293(3) 0.0297(11) Uani 1 1 d .
H26 H -0.2216 -0.4180 -0.2437 0.036 Uiso 1 1 calc R
C28 C -0.5605(6) -0.4021(5) -0.2600(3) 0.0314(11) Uani 1 1 d .
H28 H -0.6490 -0.4172 -0.2959 0.038 Uiso 1 1 calc R
O8 O -0.4204(5) 0.3028(4) 0.4912(3) 0.0534(12) Uani 1 1 d .
C27 C -0.4343(5) -0.4214(5) -0.2837(3) 0.0268(10) Uani 1 1 d .
C1 C -0.1042(6) 0.3239(5) 0.3785(3) 0.0343(12) Uani 1 1 d .
C29 C -0.5571(6) -0.3610(5) -0.1844(3) 0.0342(12) Uani 1 1 d .
H29 H -0.6441 -0.3495 -0.1680 0.041 Uiso 1 1 calc R
C11 C -0.2135(6) -0.3155(5) 0.0284(3) 0.0313(11) Uani 1 1 d .
C15 C 0.1244(6) -0.1005(5) 0.1588(3) 0.0363(12) Uani 1 1 d .
H15A H 0.1624 -0.1621 0.1714 0.055 Uiso 1 1 calc R
H15B H 0.1091 -0.0482 0.2047 0.055 Uiso 1 1 calc R
H15C H 0.1947 -0.0586 0.1374 0.055 Uiso 1 1 calc R
C21 C -0.1309(6) -0.3657(5) 0.2736(3) 0.0341(12) Uani 1 1 d .
H21 H -0.2205 -0.3686 0.2899 0.041 Uiso 1 1 calc R
C20 C -0.0104(6) -0.3748(5) 0.3187(3) 0.0333(12) Uani 1 1 d .
C17 C 0.0091(6) -0.3455(5) 0.1011(3) 0.0323(11) Uani 1 1 d .
H17A H 0.1120 -0.3198 0.0983 0.039 Uiso 1 1 calc R
H17B H -0.0296 -0.4237 0.0654 0.039 Uiso 1 1 calc R
C6 C 0.0579(7) 0.2368(5) 0.2966(4) 0.0393(13) Uani 1 1 d .
H6 H 0.1412 0.2775 0.3357 0.047 Uiso 1 1 calc R
C25 C -0.3110(6) -0.3585(5) -0.1541(3) 0.0333(12) Uani 1 1 d .
H25 H -0.2250 -0.3440 -0.1166 0.040 Uiso 1 1 calc R
C5 C 0.0738(7) 0.1708(5) 0.2288(3) 0.0381(13) Uani 1 1 d .
H5 H 0.1691 0.1682 0.2203 0.046 Uiso 1 1 calc R
C7 C -0.0245(7) 0.0458(5) 0.0971(3) 0.0345(12) Uani 1 1 d .
H7A H -0.0679 0.0789 0.0595 0.041 Uiso 1 1 calc R
H7B H 0.0811 0.0560 0.0975 0.041 Uiso 1 1 calc R
C19 C 0.1207(7) -0.3688(6) 0.2940(4) 0.0418(14) Uani 1 1 d .
H19 H 0.2061 -0.3737 0.3252 0.050 Uiso 1 1 calc R
C18 C 0.1254(7) -0.3558(6) 0.2243(4) 0.0434(15) Uani 1 1 d .
H18 H 0.2136 -0.3524 0.2066 0.052 Uiso 1 1 calc R
C22 C -0.1227(6) -0.3523(5) 0.2039(3) 0.0321(11) Uani 1 1 d .
H22 H -0.2064 -0.3460 0.1722 0.039 Uiso 1 1 calc R
C3 C -0.2007(6) 0.1771(5) 0.2516(3) 0.0367(13) Uani 1 1 d .
H3 H -0.2967 0.1778 0.2594 0.044 Uiso 1 1 calc R
C14 C -0.3133(9) -0.0520(8) -0.0112(3) 0.054(2) Uani 1 1 d .
H14A H -0.3988 -0.0456 0.0112 0.081 Uiso 1 1 calc R
H14B H -0.3455 -0.0882 -0.0659 0.081 Uiso 1 1 calc R
H14C H -0.2508 0.0243 -0.0006 0.081 Uiso 1 1 calc R
C4 C -0.1785(7) 0.1095(5) 0.1840(3) 0.0365(12) Uani 1 1 d .
H4 H -0.2598 0.0632 0.1451 0.044 Uiso 1 1 calc R
C24 C -0.4383(6) -0.2928(5) -0.0497(3) 0.0331(6) Uani 1 1 d .
H24A H -0.4947 -0.2331 -0.0429 0.040 Uiso 1 1 calc R
H24B H -0.4904 -0.3563 -0.0349 0.040 Uiso 1 1 calc R
C16 C -0.2763(8) -0.4432(7) 0.0033(4) 0.057(2) Uani 1 1 d .
H16A H -0.2036 -0.4828 -0.0158 0.086 Uiso 1 1 calc R
H16B H -0.3641 -0.4632 -0.0368 0.086 Uiso 1 1 calc R
H16C H -0.3017 -0.4661 0.0462 0.086 Uiso 1 1 calc R
O4 O 0.1067(4) -0.3745(4) 0.4386(2) 0.0373(9) Uani 1 1 d .
C23 C -0.0155(6) -0.3941(5) 0.3951(3) 0.0331(6) Uani 1 1 d .
O7 O -0.2785(5) 0.6773(4) 0.5261(3) 0.0472(11) Uani 1 1 d .
Cl1 Cl -0.5006(3) -0.3583(3) 0.1779(2) 0.1159(12) Uani 1 1 d .
N5 N -0.0987(5) 0.3391(5) 0.1022(3) 0.0331(6) Uani 1 1 d .
O11 O -0.5976(5) 0.1346(4) 0.2116(3) 0.0500(11) Uani 1 1 d .
O9 O -0.5086(10) 0.0526(9) 0.2875(6) 0.120(2) Uani 1 1 d .
O10 O -0.6217(7) 0.1830(8) 0.3285(3) 0.092(3) Uani 1 1 d .
N4 N -0.5787(8) 0.1271(6) 0.2758(5) 0.0628(17) Uani 1 1 d .
O12 O -0.101(4) 0.3873(13) 0.0775(9) 0.57(4) Uani 1 1 d .
O14 O -0.0567(10) 0.3707(9) 0.1692(6) 0.120(2) Uani 1 1 d .
O13 O -0.2198(9) 0.2522(9) 0.0727(4) 0.106(3) 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'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -2.4164 10.2820 '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 Pr1 O4 143.06(15) 2_455 2_556
O6 Pr1 O2 144.95(15) 2_455 2_566
O4 Pr1 O2 71.84(14) 2_556 2_566
O6 Pr1 O5 100.14(12) 2_455 1_566
O4 Pr1 O5 76.78(13) 2_556 1_566
O2 Pr1 O5 82.73(13) 2_566 1_566
O6 Pr1 O3 79.13(13) 2_455 1_565
O4 Pr1 O3 124.09(13) 2_556 1_565
O2 Pr1 O3 79.25(15) 2_566 1_565
O5 Pr1 O3 145.18(16) 1_566 1_565
O6 Pr1 O7 73.01(15) 2_455 .
O4 Pr1 O7 137.27(15) 2_556 .
O2 Pr1 O7 74.45(14) 2_566 .
O5 Pr1 O7 73.57(16) 1_566 .
O3 Pr1 O7 73.00(16) 1_565 .
O6 Pr1 O1 78.95(14) 2_455 .
O4 Pr1 O1 80.91(15) 2_556 .
O2 Pr1 O1 120.57(13) 2_566 .
O5 Pr1 O1 140.32(15) 1_566 .
O3 Pr1 O1 74.19(16) 1_565 .
O7 Pr1 O1 140.03(16) . .
O6 Pr1 O8 71.90(16) 2_455 .
O4 Pr1 O8 72.20(15) 2_556 .
O2 Pr1 O8 139.86(16) 2_566 .
O5 Pr1 O8 72.22(16) 1_566 .
O3 Pr1 O8 137.18(17) 1_565 .
O7 Pr1 O8 124.71(16) . .
O1 Pr1 O8 69.88(16) . .
C30 O6 Pr1 176.8(3) . 2_455
C30 O5 Pr1 130.2(3) . 1_544
C22 N2 C18 122.7(5) . .
C22 N2 C17 119.5(5) . .
C18 N2 C17 117.5(4) . .
C25 N3 C29 121.5(5) . .
C25 N3 C24 120.9(5) . .
C29 N3 C24 117.4(4) . .
C4 N1 C5 121.5(5) . .
C4 N1 C7 117.8(5) . .
C5 N1 C7 120.5(5) . .
C1 O1 Pr1 108.6(3) . .
C13 C8 C9 121.0(5) . .
C13 C8 C7 120.4(5) . .
C9 C8 C7 118.6(5) . .
C10 C9 C8 120.5(5) . .
C10 C9 C15 119.2(5) . .
C8 C9 C15 120.4(5) . .
O6 C30 O5 126.2(5) . .
O6 C30 C27 117.8(4) . .
O5 C30 C27 116.0(4) . .
C1 O2 Pr1 173.8(4) . 2_566
C9 C10 C11 120.2(5) . .
C9 C10 C17 120.7(5) . .
C11 C10 C17 119.0(5) . .
C23 O3 Pr1 135.3(4) . 1_545
C8 C13 C12 118.5(5) . .
C8 C13 C14 123.6(6) . .
C12 C13 C14 117.9(6) . .
C6 C2 C3 119.7(5) . .
C6 C2 C1 122.0(5) . .
C3 C2 C1 118.3(5) . .
C11 C12 C13 120.4(5) . .
C11 C12 C24 120.3(5) . .
C13 C12 C24 119.3(5) . .
C25 C26 C27 119.4(5) . .
C29 C28 C27 119.7(5) . .
C28 C27 C26 118.3(5) . .
C28 C27 C30 121.3(5) . .
C26 C27 C30 120.4(4) . .
O1 C1 O2 124.8(5) . .
O1 C1 C2 117.7(5) . .
O2 C1 C2 117.5(5) . .
N3 C29 C28 120.5(5) . .
C10 C11 C12 119.4(5) . .
C10 C11 C16 120.1(6) . .
C12 C11 C16 120.4(6) . .
C20 C21 C22 120.0(5) . .
C21 C20 C19 119.1(5) . .
C21 C20 C23 121.8(5) . .
C19 C20 C23 119.0(5) . .
C10 C17 N2 112.2(4) . .
C5 C6 C2 119.3(6) . .
N3 C25 C26 120.5(5) . .
N1 C5 C6 120.9(5) . .
C8 C7 N1 113.1(4) . .
C18 C19 C20 119.6(6) . .
N2 C18 C19 119.1(5) . .
N2 C22 C21 119.5(5) . .
C2 C3 C4 118.6(5) . .
N1 C4 C3 119.8(6) . .
C12 C24 N3 113.0(4) . .
C23 O4 Pr1 135.5(4) . 2_556
O3 C23 O4 128.6(5) . .
O3 C23 C20 116.1(5) . .
O4 C23 C20 115.3(5) . .
O12 N5 O14 120.9(12) . .
O12 N5 O13 109(2) . .
O14 N5 O13 117.0(7) . .
O10 N4 O11 125.6(8) . .
O10 N4 O9 118.0(9) . .
O11 N4 O9 116.3(8) . .
N5 O12 O14 34.9(8) . .
N5 O14 O12 24.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 O6 2.385(4) 2_455
Pr1 O4 2.420(4) 2_556
Pr1 O2 2.429(4) 2_566
Pr1 O5 2.466(3) 1_566
Pr1 O3 2.481(4) 1_565
Pr1 O7 2.485(5) .
Pr1 O1 2.489(4) .
Pr1 O8 2.568(5) .
O6 C30 1.235(6) .
O6 Pr1 2.385(4) 2_455
O5 C30 1.253(6) .
O5 Pr1 2.466(3) 1_544
N2 C22 1.331(7) .
N2 C18 1.342(8) .
N2 C17 1.538(6) .
N3 C25 1.326(7) .
N3 C29 1.332(7) .
N3 C24 1.542(7) .
N1 C4 1.333(7) .
N1 C5 1.338(8) .
N1 C7 1.508(7) .
O1 C1 1.250(7) .
C8 C13 1.381(8) .
C8 C9 1.397(8) .
C8 C7 1.506(8) .
C9 C10 1.390(7) .
C9 C15 1.521(7) .
C30 C27 1.525(6) .
O2 C1 1.255(7) .
O2 Pr1 2.429(4) 2_566
C10 C11 1.397(7) .
C10 C17 1.492(8) .
O3 C23 1.242(7) .
O3 Pr1 2.481(4) 1_545
C13 C12 1.432(9) .
C13 C14 1.524(8) .
C2 C6 1.368(8) .
C2 C3 1.390(8) .
C2 C1 1.523(7) .
C12 C11 1.401(9) .
C12 C24 1.498(8) .
C26 C25 1.379(7) .
C26 C27 1.388(7) .
C28 C29 1.371(7) .
C28 C27 1.385(7) .
C11 C16 1.514(9) .
C21 C20 1.363(8) .
C21 C22 1.382(8) .
C20 C19 1.395(7) .
C20 C23 1.533(7) .
C6 C5 1.367(8) .
C19 C18 1.376(9) .
C3 C4 1.395(8) .
O4 C23 1.258(7) .
O4 Pr1 2.420(4) 2_556
N5 O12 0.858(16) .
N5 O14 1.195(11) .
N5 O13 1.357(10) .
O11 N4 1.229(9) .
O9 N4 1.289(12) .
O10 N4 1.223(9) .
O12 O14 1.794(17) .
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 0.028 0.000 0.500 563.0 154.4
