#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:17:09 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143498 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/52/7035246.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_7035246
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 La N5 O14'
_chemical_formula_weight         855.93
_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                106.1310(10)
_cell_angle_beta                 98.9710(10)
_cell_angle_gamma                100.4790(10)
_cell_formula_units_Z            2
_cell_length_a                   9.55740(10)
_cell_length_b                   12.6056(2)
_cell_length_c                   18.9892(3)
_cell_measurement_reflns_used    11263
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0480
_cell_measurement_theta_min      3.1060
_cell_volume                     2108.78(6)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28175
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.914
_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    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.029
_platon_squeeze_details
;
;
_refine_diff_density_max         1.945
_refine_diff_density_min         -2.558
_refine_diff_density_rms         0.161
_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     447
_refine_ls_number_reflns         10138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1105P)²+5.0822P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1841
_reflns_number_gt                8730
_reflns_number_total             10138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01598g2.cif
_cod_data_source_block           la_final
_cod_depositor_comments
'Adding full bibliography for 7035246--7035254.cif.'
_cod_original_cell_volume        2108.78(5)
_cod_database_code               7035246
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
La1 La -0.23318(3) -0.01821(2) -0.003855(13) 0.02508(11) Uani 1 1 d .
O1 O -0.3095(4) 0.0227(4) 0.11957(19) 0.0360(8) Uani 1 1 d .
O2 O -0.5402(4) 0.0311(3) 0.08820(19) 0.0335(8) Uani 1 1 d .
N2 N 0.0004(5) 0.1475(4) 0.6786(2) 0.0284(8) Uani 1 1 d .
O5 O -0.0025(4) 0.8890(3) 0.9256(2) 0.0342(8) Uani 1 1 d .
O6 O -0.2394(4) 0.8140(4) 0.8833(2) 0.0436(10) Uani 1 1 d .
O4 O -0.1421(4) 0.0673(4) 0.9013(2) 0.0409(9) Uani 1 1 d .
N3 N -0.0428(5) 0.6089(4) 0.6747(2) 0.0325(9) Uani 1 1 d .
O3 O 0.1026(4) 0.1239(4) 0.9354(2) 0.0378(8) Uani 1 1 d .
C10 C -0.0780(5) 0.2322(4) 0.5775(3) 0.0266(9) Uani 1 1 d .
C11 C -0.0191(5) 0.3483(4) 0.6023(2) 0.0273(9) Uani 1 1 d .
C8 C -0.2875(5) 0.2588(5) 0.5016(3) 0.0352(12) Uani 1 1 d .
C12 C -0.0914(5) 0.4200(4) 0.5747(3) 0.0287(9) Uani 1 1 d .
O8 O -0.2776(5) 0.1809(4) 0.0271(3) 0.0496(11) Uani 1 1 d .
C2 C -0.4319(5) 0.0809(4) 0.2171(3) 0.0271(9) Uani 1 1 d .
C13 C -0.2265(6) 0.3749(5) 0.5228(3) 0.0345(11) Uani 1 1 d .
C4 C -0.5566(5) 0.1403(5) 0.3159(3) 0.0336(11) Uani 1 1 d .
H4 H -0.6439 0.1513 0.3317 0.040 Uiso 1 1 calc R
O9 O 0.4004(9) -0.3668(7) -0.2887(5) 0.1003(16) Uani 1 1 d .
C3 C -0.5579(5) 0.0992(5) 0.2406(3) 0.0325(11) Uani 1 1 d .
H3 H -0.6460 0.0833 0.2044 0.039 Uiso 1 1 calc R
C9 C -0.2160(5) 0.1852(5) 0.5272(3) 0.0314(10) Uani 1 1 d .
C20 C -0.0120(6) 0.1227(5) 0.8160(3) 0.0341(11) Uani 1 1 d .
C6 C -0.3049(5) 0.1021(5) 0.2719(3) 0.0306(10) Uani 1 1 d .
H6 H -0.2177 0.0869 0.2578 0.037 Uiso 1 1 calc R
C18 C -0.1255(5) 0.1451(5) 0.7016(3) 0.0323(10) Uani 1 1 d .
H18 H -0.2083 0.1534 0.6707 0.039 Uiso 1 1 calc R
C23 C -0.0180(6) 0.1033(5) 0.8914(3) 0.0361(11) Uani 1 1 d .
C5 C -0.3083(5) 0.1454(5) 0.3466(3) 0.0328(11) Uani 1 1 d .
H5 H -0.2221 0.1614 0.3840 0.039 Uiso 1 1 calc R
C1 C -0.4280(5) 0.0404(4) 0.1343(3) 0.0280(9) Uani 1 1 d .
C16 C 0.1241(6) 0.3975(5) 0.6595(3) 0.0372(11) Uani 1 1 d .
H16A H 0.1463 0.3407 0.6830 0.056 Uiso 1 1 calc R
H16B H 0.1167 0.4652 0.6981 0.056 Uiso 1 1 calc R
H16C H 0.2021 0.4184 0.6344 0.056 Uiso 1 1 calc R
C19 C -0.1345(6) 0.1305(5) 0.7701(3) 0.0343(11) Uani 1 1 d .
H19 H -0.2245 0.1259 0.7858 0.041 Uiso 1 1 calc R
C17 C 0.0074(6) 0.1533(4) 0.6003(3) 0.0323(10) Uani 1 1 d .
H17A H 0.1106 0.1792 0.5984 0.039 Uiso 1 1 calc R
H17B H -0.0309 0.0761 0.5637 0.039 Uiso 1 1 calc R
C21 C 0.1171(6) 0.1281(6) 0.7908(4) 0.0424(13) Uani 1 1 d .
H21 H 0.2029 0.1238 0.8217 0.051 Uiso 1 1 calc R
C27 C -0.0835(6) 0.7410(4) 0.8079(3) 0.0334(11) Uani 1 1 d .
C26 C 0.0559(6) 0.7371(5) 0.7975(3) 0.0385(12) Uani 1 1 d .
H26 H 0.1384 0.7798 0.8365 0.046 Uiso 1 1 calc R
C24 C -0.0203(7) 0.5463(5) 0.5998(3) 0.0378(12) Uani 1 1 d .
H24A H 0.0857 0.5565 0.6020 0.045 Uiso 1 1 calc R
H24B H -0.0608 0.5795 0.5620 0.045 Uiso 1 1 calc R
O7 O -0.4221(5) -0.1971(4) -0.0069(3) 0.0577(13) Uani 1 1 d .
C30 C -0.1102(6) 0.8196(5) 0.8777(3) 0.0355(11) Uani 1 1 d .
C29 C -0.1774(6) 0.6086(5) 0.6851(3) 0.0381(12) Uani 1 1 d .
H29 H -0.2583 0.5623 0.6462 0.046 Uiso 1 1 calc R
C15 C -0.2789(8) 0.0594(6) 0.5017(4) 0.0597(19) Uani 1 1 d .
H15A H -0.3640 0.0394 0.4603 0.090 Uiso 1 1 calc R
H15B H -0.3086 0.0368 0.5436 0.090 Uiso 1 1 calc R
H15C H -0.2053 0.0196 0.4847 0.090 Uiso 1 1 calc R
C28 C -0.2014(6) 0.6740(5) 0.7511(3) 0.0393(12) Uani 1 1 d .
H28 H -0.2981 0.6732 0.7576 0.047 Uiso 1 1 calc R
C22 C 0.1207(6) 0.1396(5) 0.7213(4) 0.0406(13) Uani 1 1 d .
H22 H 0.2085 0.1418 0.7035 0.049 Uiso 1 1 calc R
C7 C -0.4373(6) 0.2091(7) 0.4492(3) 0.0485(16) Uani 1 1 d .
H7A H -0.4898 0.1461 0.4638 0.058 Uiso 1 1 calc R
H7B H -0.4937 0.2684 0.4555 0.058 Uiso 1 1 calc R
C25 C 0.0738(6) 0.6709(5) 0.7303(3) 0.0394(12) Uani 1 1 d .
H25 H 0.1694 0.6685 0.7228 0.047 Uiso 1 1 calc R
C14 C -0.3082(8) 0.4504(7) 0.4897(3) 0.0532(17) Uani 1 1 d .
H14A H -0.3403 0.4153 0.4351 0.080 Uiso 1 1 calc R
H14B H -0.2431 0.5255 0.5011 0.080 Uiso 1 1 calc R
H14C H -0.3933 0.4584 0.5117 0.080 Uiso 1 1 calc R
N5 N 0.4224(12) -0.3717(9) -0.2282(6) 0.102(3) Uani 1 1 d .
O10 O 0.3844(9) -0.3111(7) -0.1717(5) 0.1003(16) Uani 1 1 d .
Cl1 Cl -0.4964(4) -0.1352(3) 0.3197(2) 0.1211(11) Uiso 1 1 d .
N4 N -0.1002(4) -0.1603(4) 0.6020(3) 0.0268(9) Uani 1 1 d .
O13 O -0.2155(10) -0.211(2) 0.5762(5) 0.341(16) Uani 1 1 d .
O12 O -0.0424(14) -0.1547(15) 0.6559(12) 0.269(12) Uani 1 1 d .
O14 O -0.0152(18) -0.1215(13) 0.5761(7) 0.192(6) Uani 1 1 d .
N1 N -0.4307(5) 0.1650(4) 0.3671(2) 0.0331(9) Uani 1 1 d .
O11 O 0.4853(11) -0.4520(9) -0.2152(6) 0.124(3) Uiso 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'
Cl Cl 0.1484 0.1585 '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'
La La -0.2871 2.4523 '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'
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
O2 La1 O3 143.70(14) 2_455 2_556
O2 La1 O5 144.82(13) 2_455 2_566
O3 La1 O5 71.35(13) 2_556 2_566
O2 La1 O1 100.68(11) 2_455 .
O3 La1 O1 75.71(12) 2_556 .
O5 La1 O1 83.04(12) 2_566 .
O2 La1 O4 77.97(12) 2_455 1_554
O3 La1 O4 125.35(12) 2_556 1_554
O5 La1 O4 79.57(13) 2_566 1_554
O1 La1 O4 145.18(14) . 1_554
O2 La1 O6 77.94(12) 2_455 1_544
O3 La1 O6 82.45(14) 2_556 1_544
O5 La1 O6 121.06(12) 2_566 1_544
O1 La1 O6 139.98(15) . 1_544
O4 La1 O6 74.37(15) 1_554 1_544
O2 La1 O8 73.27(13) 2_455 .
O3 La1 O8 135.83(14) 2_556 .
O5 La1 O8 74.53(13) 2_566 .
O1 La1 O8 73.05(15) . .
O4 La1 O8 73.33(15) 1_554 .
O6 La1 O8 140.29(15) 1_544 .
O2 La1 O7 72.05(14) 2_455 .
O3 La1 O7 72.57(14) 2_556 .
O5 La1 O7 140.07(15) 2_566 .
O1 La1 O7 71.97(16) . .
O4 La1 O7 136.88(16) 1_554 .
O6 La1 O7 69.63(16) 1_544 .
O8 La1 O7 124.07(15) . .
O2 La1 O5 116.98(10) 2_455 1_544
O3 La1 O5 65.19(12) 2_556 1_544
O5 La1 O5 74.93(12) 2_566 1_544
O1 La1 O5 139.44(11) . 1_544
O4 La1 O5 63.03(12) 1_554 1_544
O6 La1 O5 46.13(11) 1_544 1_544
O8 La1 O5 130.12(14) . 1_544
O7 La1 O5 104.56(13) . 1_544
O2 La1 C30 96.48(13) 2_455 1_544
O3 La1 C30 74.02(14) 2_556 1_544
O5 La1 C30 98.53(13) 2_566 1_544
O1 La1 C30 147.35(14) . 1_544
O4 La1 C30 65.71(15) 1_554 1_544
O6 La1 C30 22.56(13) 1_544 1_544
O8 La1 C30 139.03(16) . 1_544
O7 La1 C30 87.44(16) . 1_544
O5 La1 C30 23.64(11) 1_544 1_544
C1 O1 La1 129.5(3) . .
C1 O2 La1 176.5(3) . 2_455
C22 N2 C18 122.0(4) . .
C22 N2 C17 117.8(4) . .
C18 N2 C17 120.1(4) . .
C30 O5 La1 170.6(3) . 2_566
C30 O5 La1 83.7(3) . 1_566
La1 O5 La1 105.07(12) 2_566 1_566
C30 O6 La1 106.0(3) . 1_566
C23 O4 La1 134.0(3) . 1_556
C29 N3 C25 120.4(4) . .
C29 N3 C24 119.9(5) . .
C25 N3 C24 119.7(4) . .
C23 O3 La1 136.0(4) . 2_556
C11 C10 C9 120.6(5) . .
C11 C10 C17 120.3(4) . .
C9 C10 C17 119.0(5) . .
C10 C11 C12 120.2(4) . .
C10 C11 C16 119.8(5) . .
C12 C11 C16 120.0(5) . .
C13 C8 C9 122.1(5) . .
C13 C8 C7 119.7(5) . .
C9 C8 C7 118.2(5) . .
C11 C12 C13 120.2(5) . .
C11 C12 C24 119.0(5) . .
C13 C12 C24 120.8(5) . .
C3 C2 C6 118.2(4) . .
C3 C2 C1 121.9(4) . .
C6 C2 C1 119.9(4) . .
C8 C13 C12 118.7(5) . .
C8 C13 C14 119.4(5) . .
C12 C13 C14 121.9(6) . .
N1 C4 C3 119.7(4) . .
C4 C3 C2 120.5(4) . .
C8 C9 C10 118.1(5) . .
C8 C9 C15 122.1(5) . .
C10 C9 C15 119.8(6) . .
C19 C20 C21 118.7(5) . .
C19 C20 C23 121.4(5) . .
C21 C20 C23 119.8(5) . .
C5 C6 C2 119.1(4) . .
N2 C18 C19 119.9(5) . .
O3 C23 O4 128.0(5) . .
O3 C23 C20 115.6(5) . .
O4 C23 C20 116.4(5) . .
N1 C5 C6 121.0(4) . .
O2 C1 O1 126.3(4) . .
O2 C1 C2 117.3(4) . .
O1 C1 C2 116.4(4) . .
C18 C19 C20 119.7(5) . .
C10 C17 N2 113.0(4) . .
C22 C21 C20 119.9(5) . .
C28 C27 C26 118.8(5) . .
C28 C27 C30 119.2(5) . .
C26 C27 C30 122.0(5) . .
C25 C26 C27 119.4(5) . .
N3 C24 C12 113.0(4) . .
O6 C30 O5 123.9(5) . .
O6 C30 C27 117.3(5) . .
O5 C30 C27 118.8(4) . .
O6 C30 La1 51.5(3) . 1_566
O5 C30 La1 72.7(3) . 1_566
C27 C30 La1 166.3(4) . 1_566
N3 C29 C28 121.2(5) . .
C29 C28 C27 119.4(5) . .
N2 C22 C21 119.8(5) . .
N1 C7 C8 113.2(4) . .
N3 C25 C26 120.7(5) . .
O9 N5 O10 126.6(11) . .
O9 N5 O11 118.4(11) . .
O10 N5 O11 114.9(9) . .
O12 N4 O13 123.8(11) . .
O12 N4 O14 104.5(11) . .
O13 N4 O14 130.6(10) . .
C5 N1 C4 121.3(4) . .
C5 N1 C7 121.6(4) . .
C4 N1 C7 117.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O2 2.435(3) 2_455
La1 O3 2.466(4) 2_556
La1 O5 2.493(3) 2_566
La1 O1 2.508(3) .
La1 O4 2.527(4) 1_554
La1 O6 2.542(4) 1_544
La1 O8 2.544(4) .
La1 O7 2.601(5) .
La1 O5 3.002(4) 1_544
La1 C30 3.124(5) 1_544
O1 C1 1.252(6) .
O2 C1 1.240(6) .
O2 La1 2.435(3) 2_455
N2 C22 1.336(7) .
N2 C18 1.341(6) .
N2 C17 1.521(6) .
O5 C30 1.261(6) .
O5 La1 2.493(3) 2_566
O5 La1 3.002(4) 1_566
O6 C30 1.247(6) .
O6 La1 2.542(4) 1_566
O4 C23 1.253(7) .
O4 La1 2.527(4) 1_556
N3 C29 1.331(7) .
N3 C25 1.351(7) .
N3 C24 1.492(6) .
O3 C23 1.251(6) .
O3 La1 2.466(4) 2_556
C10 C11 1.385(7) .
C10 C9 1.419(6) .
C10 C17 1.504(7) .
C11 C12 1.394(7) .
C11 C16 1.514(7) .
C8 C13 1.390(8) .
C8 C9 1.393(8) .
C8 C7 1.522(7) .
C12 C13 1.410(7) .
C12 C24 1.518(8) .
C2 C3 1.383(6) .
C2 C6 1.401(6) .
C2 C1 1.520(6) .
C13 C14 1.536(8) .
C4 N1 1.350(6) .
C4 C3 1.376(7) .
O9 N5 1.156(11) .
C9 C15 1.499(8) .
C20 C19 1.383(7) .
C20 C21 1.388(7) .
C20 C23 1.526(7) .
C6 C5 1.379(7) .
C18 C19 1.376(7) .
C5 N1 1.333(6) .
C21 C22 1.373(8) .
C27 C28 1.385(7) .
C27 C26 1.385(7) .
C27 C30 1.507(7) .
C26 C25 1.371(8) .
C30 La1 3.124(5) 1_566
C29 C28 1.373(7) .
C7 N1 1.518(6) .
N5 O10 1.278(12) .
N5 O11 1.327(13) .
N4 O12 1.063(16) .
N4 O13 1.125(14) .
N4 O14 1.120(19) .
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 0.002 0.500 0.000 596.6 10.1
