#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:50:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179396 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/93/4329369.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_4329369
loop_
_publ_author_name
'Manolis J. Manos'
'Eleni J. Kyprianidou'
'Giannis S. Papaefstathiou'
'Anastasios J. Tasiopoulos'
_publ_section_title
;
 Insertion of Functional Groups into a Nd3+ Metal-Organic Framework via
 Single-Crystal-to-Single-Crystal Coordinating Solvent Exchange
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6308
_journal_page_last               6314
_journal_paper_doi               10.1021/ic3005085
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C32 H16 Cl N2 Nd2 O15, C3 H3 N2'
_chemical_formula_sum            'C35 H19 Cl N4 Nd2 O15'
_chemical_formula_weight         1059.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.997(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.5336(16)
_cell_length_b                   14.7711(8)
_cell_length_c                   13.6945(9)
_cell_measurement_reflns_used    3868
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8781
_cell_measurement_theta_min      3.0063
_cell_volume                     5700.8(6)
_computing_cell_refinement       'CrysAlis RED'
_computing_data_collection       'CrysAlis CCD'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
;
 DIAMOND (Brandenburg, 2006)
 MERCURY (Bruno et al. 2002)
;
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11380
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.653
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4986
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1053P)²+0.5896P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1736
_reflns_number_gt                3740
_reflns_number_total             4986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3005085_si_002_07.cif
_cod_data_source_block           UCY-2-Cl
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4329369
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Nd1 Nd 0.181713(12) 0.21156(2) 0.46041(3) 0.02536(18) Uani 1 1 d U
O1 O 0.1128(2) 0.1857(4) 0.5535(5) 0.0549(16) Uani 1 1 d U
O2 O 0.1126(2) 0.3134(4) 0.4701(5) 0.0549(17) Uani 1 1 d U
O3 O 0.20499(18) 0.0781(3) 0.5673(4) 0.0457(14) Uani 1 1 d U
O4 O 0.23346(17) 0.3379(3) 0.4455(4) 0.0357(12) Uani 1 1 d U
O5 O 0.1991(2) 0.2879(3) 0.6187(4) 0.0413(14) Uani 1 1 d U
O6 O 0.23117(18) 0.1430(4) 0.3511(4) 0.0453(14) Uani 1 1 d U
O7 O 0.1516(3) 0.2737(5) 0.2852(6) 0.074(2) Uani 1 1 d U
Cl1 Cl 0.1186(4) 0.0850(12) 0.3655(11) 0.112(4) Uani 0.50 1 d PU
O8 O 0.1396(10) 0.085(3) 0.371(3) 0.134(14) Uani 0.50 1 d PU
N1 N -0.0971(2) 0.4381(5) 0.6538(5) 0.0450(17) Uani 1 1 d U
N2 N 0.0372(11) 0.2985(17) 0.2828(19) 0.284(16) Uani 1 1 d DU
C1 C 0.0947(3) 0.2610(6) 0.5276(6) 0.043(2) Uani 1 1 d U
C2 C 0.0511(3) 0.2878(5) 0.5663(6) 0.0398(19) Uani 1 1 d U
C3 C 0.0230(4) 0.2237(7) 0.6018(9) 0.066(3) Uani 1 1 d U
H3 H 0.0327 0.1635 0.6059 0.079 Uiso 1 1 calc R
C4 C -0.0194(4) 0.2478(7) 0.6315(9) 0.070(3) Uani 1 1 d U
H4 H -0.0384 0.2037 0.6541 0.084 Uiso 1 1 calc R
C5 C -0.0336(3) 0.3368(6) 0.6277(6) 0.044(2) Uani 1 1 d U
C6 C -0.0051(3) 0.4022(6) 0.5938(6) 0.045(2) Uani 1 1 d U
H6 H -0.0142 0.4627 0.5927 0.055 Uiso 1 1 calc R
C7 C 0.0365(3) 0.3784(6) 0.5618(6) 0.050(2) Uani 1 1 d U
H7 H 0.0549 0.4223 0.5373 0.060 Uiso 1 1 calc R
C8 C -0.0801(3) 0.3580(6) 0.6557(6) 0.047(2) Uani 1 1 d DU
H16 H -0.094(4) 0.299(4) 0.677(8) 0.09(4) Uiso 1 1 d D
C9 C 0.2483(3) 0.0921(5) 0.5852(5) 0.0344(17) Uani 1 1 d U
C10 C 0.2803(3) 0.0237(5) 0.6429(5) 0.0352(17) Uani 1 1 d U
C11 C 0.3271(3) 0.0150(5) 0.6274(5) 0.0375(18) Uani 1 1 d U
H11 H 0.3391 0.0537 0.5838 0.045 Uiso 1 1 calc R
C12 C 0.3561(3) -0.0522(5) 0.6778(6) 0.0377(18) Uani 1 1 d U
C13 C 0.3387(3) -0.1062(5) 0.7472(5) 0.0390(19) Uani 1 1 d U
H13 H 0.3583 -0.1488 0.7832 0.047 Uiso 1 1 calc R
C14 C 0.2919(3) -0.0967(5) 0.7629(5) 0.0340(17) Uani 1 1 d U
C15 C 0.2625(3) -0.0326(5) 0.7096(5) 0.0342(17) Uani 1 1 d U
H15 H 0.2310 -0.0274 0.7187 0.041 Uiso 1 1 calc R
C16 C 0.2275(3) 0.3438(5) 0.6627(5) 0.0387(18) Uani 1 1 d U
C17 C 0.0000 0.241(3) 0.2500 0.26(2) Uani 1 2 d SDU
H17 H 0.0000 0.1776 0.2500 0.312 Uiso 1 2 calc SR
C18 C 0.0238(7) 0.3854(13) 0.2637(18) 0.161(10) Uani 1 1 d DU
H18 H 0.0437 0.4357 0.2684 0.193 Uiso 1 1 calc R
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'
Nd Nd -0.1943 3.0179 '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'
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
O4 Nd1 O5 70.90(17) . .
O4 Nd1 O6 81.25(17) . .
O5 Nd1 O6 133.32(19) . .
O4 Nd1 O8 144.0(10) . .
O5 Nd1 O8 145.1(10) . .
O6 Nd1 O8 70.1(7) . .
O4 Nd1 O3 123.65(18) . .
O5 Nd1 O3 81.01(19) . .
O6 Nd1 O3 84.54(19) . .
O8 Nd1 O3 75.8(12) . .
O4 Nd1 O2 92.14(19) . .
O5 Nd1 O2 74.1(2) . .
O6 Nd1 O2 145.2(2) . .
O8 Nd1 O2 99.1(8) . .
O3 Nd1 O2 125.94(18) . .
O4 Nd1 O1 133.96(18) . .
O5 Nd1 O1 71.8(2) . .
O6 Nd1 O1 144.79(18) . .
O8 Nd1 O1 77.2(7) . .
O3 Nd1 O1 74.97(17) . .
O2 Nd1 O1 51.96(18) . .
O4 Nd1 O7 76.4(2) . .
O5 Nd1 O7 131.0(2) . .
O6 Nd1 O7 73.6(2) . .
O8 Nd1 O7 74.9(12) . .
O3 Nd1 O7 148.0(2) . .
O2 Nd1 O7 71.7(2) . .
O1 Nd1 O7 110.4(2) . .
O4 Nd1 O4 74.35(17) . 7_556
O5 Nd1 O4 69.57(18) . 7_556
O6 Nd1 O4 67.20(17) . 7_556
O8 Nd1 O4 111.8(10) . 7_556
O3 Nd1 O4 50.00(16) . 7_556
O2 Nd1 O4 143.6(2) . 7_556
O1 Nd1 O4 115.70(18) . 7_556
O7 Nd1 O4 133.8(2) . 7_556
O4 Nd1 Cl1 147.6(3) . .
O5 Nd1 Cl1 139.4(3) . .
O6 Nd1 Cl1 80.1(3) . .
O8 Nd1 Cl1 10.9(9) . .
O3 Nd1 Cl1 80.6(4) . .
O2 Nd1 Cl1 88.3(4) . .
O1 Nd1 Cl1 68.6(3) . .
O7 Nd1 Cl1 73.0(4) . .
O4 Nd1 Cl1 121.1(4) 7_556 .
O4 Nd1 C1 113.7(2) . .
O5 Nd1 C1 70.2(2) . .
O6 Nd1 C1 156.4(2) . .
O8 Nd1 C1 88.5(7) . .
O3 Nd1 C1 100.2(2) . .
O2 Nd1 C1 26.1(2) . .
O1 Nd1 C1 25.8(2) . .
O7 Nd1 C1 91.6(2) . .
O4 Nd1 C1 132.9(2) 7_556 .
Cl1 Nd1 C1 77.9(3) . .
O4 Nd1 C9 99.55(19) . .
O5 Nd1 C9 74.7(2) . .
O6 Nd1 C9 73.9(2) . .
O8 Nd1 C9 93.1(11) . .
O3 Nd1 C9 24.61(18) . .
O2 Nd1 C9 140.75(19) . .
O1 Nd1 C9 95.66(19) . .
O7 Nd1 C9 147.5(2) . .
O4 Nd1 C9 25.41(18) 7_556 .
Cl1 Nd1 C9 100.4(4) . .
C1 Nd1 C9 118.6(2) . .
C1 O1 Nd1 92.4(5) . .
C1 O2 Nd1 93.6(5) . .
C9 O3 Nd1 98.7(4) . .
C9 O4 Nd1 163.0(5) 7_556 .
C9 O4 Nd1 89.7(4) 7_556 7_556
Nd1 O4 Nd1 105.65(17) . 7_556
C16 O5 Nd1 140.3(5) . .
C16 O6 Nd1 133.3(5) 7_556 .
O8 Cl1 Nd1 51(5) . .
Cl1 O8 Nd1 118(5) . .
C8 N1 C12 116.9(7) . 3_455
C18 N2 C17 110(3) . .
O1 C1 O2 122.0(7) . .
O1 C1 C2 117.9(7) . .
O2 C1 C2 120.1(7) . .
O1 C1 Nd1 61.8(4) . .
O2 C1 Nd1 60.2(4) . .
C2 C1 Nd1 177.5(6) . .
C3 C2 C7 119.0(7) . .
C3 C2 C1 120.7(7) . .
C7 C2 C1 120.1(7) . .
C2 C3 C4 120.8(9) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C5 C4 C3 120.0(9) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C6 119.7(8) . .
C4 C5 C8 117.7(8) . .
C6 C5 C8 122.6(8) . .
C7 C6 C5 120.5(8) . .
C7 C6 H6 119.7 . .
C5 C6 H6 119.7 . .
C6 C7 C2 119.9(7) . .
C6 C7 H7 120.0 . .
C2 C7 H7 120.0 . .
N1 C8 C5 123.1(8) . .
N1 C8 H16 130(6) . .
C5 C8 H16 107(6) . .
O3 C9 O4 121.5(7) . 7_556
O3 C9 C10 119.9(6) . .
O4 C9 C10 118.6(7) 7_556 .
O3 C9 Nd1 56.7(4) . .
O4 C9 Nd1 64.9(4) 7_556 .
C10 C9 Nd1 174.6(5) . .
C15 C10 C11 120.3(7) . .
C15 C10 C9 119.6(6) . .
C11 C10 C9 120.1(6) . .
C10 C11 C12 119.8(6) . .
C10 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
C13 C12 C11 119.7(6) . .
C13 C12 N1 123.1(6) . 3_545
C11 C12 N1 117.3(6) . 3_545
C14 C13 C12 120.1(6) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C13 C14 C15 120.1(6) . .
C13 C14 C16 120.3(6) . 4_546
C15 C14 C16 119.6(6) . 4_546
C10 C15 C14 120.0(6) . .
C10 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
O6 C16 O5 126.4(7) 7_556 .
O6 C16 C14 117.9(7) 7_556 4_556
O5 C16 C14 115.7(7) . 4_556
N2 C17 N2 104(4) . 2
N2 C17 H17 128.2 . .
N2 C17 H17 128.2 2 .
N2 C18 C18 107.2(17) . 2
N2 C18 H18 126.4 . .
C18 C18 H18 126.4 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nd1 O4 2.408(5) .
Nd1 O5 2.425(5) .
Nd1 O6 2.433(5) .
Nd1 O8 2.45(3) .
Nd1 O3 2.483(5) .
Nd1 O2 2.500(5) .
Nd1 O1 2.534(5) .
Nd1 O7 2.587(8) .
Nd1 O4 2.660(5) 7_556
Nd1 Cl1 2.775(14) .
Nd1 C1 2.874(8) .
Nd1 C9 2.937(7) .
O1 C1 1.254(10) .
O2 C1 1.268(10) .
O3 C9 1.237(9) .
O4 C9 1.260(9) 7_556
O4 Nd1 2.660(5) 7_556
O5 C16 1.243(9) .
O6 C16 1.240(9) 7_556
Cl1 O8 0.59(3) .
N1 C8 1.278(10) .
N1 C12 1.432(9) 3_455
N2 C18 1.353(16) .
N2 C17 1.383(18) .
C1 C2 1.479(11) .
C2 C3 1.378(12) .
C2 C7 1.400(10) .
C3 C4 1.383(13) .
C3 H3 0.9300 .
C4 C5 1.375(13) .
C4 H4 0.9300 .
C5 C6 1.388(11) .
C5 C8 1.472(11) .
C6 C7 1.373(10) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C8 H16 1.01(2) .
C9 O4 1.260(9) 7_556
C9 C10 1.502(10) .
C10 C15 1.388(9) .
C10 C11 1.391(9) .
C11 C12 1.403(10) .
C11 H11 0.9300 .
C12 C13 1.392(10) .
C12 N1 1.432(9) 3_545
C13 C14 1.392(10) .
C13 H13 0.9300 .
C14 C15 1.394(9) .
C14 C16 1.514(9) 4_546
C15 H15 0.9300 .
C16 O6 1.240(9) 7_556
C16 C14 1.514(9) 4_556
C17 N2 1.383(18) 2
C17 H17 0.9300 .
C18 C18 1.35(4) 2
C18 H18 0.9300 .
