#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:59:31 +0100 (vie 25 de mar de 2016) $
#$Revision: 179946 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/41/7024134.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_7024134
loop_
_publ_author_name
'Höller, Christoph J'
'Mai, Marit'
'Feldmann, Claus'
'Müller-Buschbaum, Klaus'
_publ_section_title
;
 The interaction of rare earth chlorides with 4,4'-bipyridine for the
 reversible formation of template based luminescent Ln-N-MOFs.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              461
_journal_page_last               468
_journal_paper_doi               10.1039/b911460b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         2-infinite[Pr2Cl6(C10H8N2)3](C10H8N2)2
_chemical_formula_sum            'C25 H20 Cl3 N5 Pr'
_chemical_formula_weight         637.72
_chemical_name_common
;2D-(Hexakis-chloro-tris-(4,4-bipyridino)-di-
praseodymium(iii))-di-4,4-bipridine
;
_chemical_name_systematic
;
2D-[Hexakis-chloro-tris-(4,4-bipyridino)-di-praseodymium(III)]-di-4,4-bipridine
;
_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                103.24(3)
_cell_angle_beta                 100.13(3)
_cell_angle_gamma                101.10(3)
_cell_formula_units_Z            2
_cell_length_a                   10.939(2)
_cell_length_b                   10.992(2)
_cell_length_c                   11.833(2)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      5.5
_cell_volume                     1322.6(5)
_computing_cell_refinement       'STOE SOFTWARE'
_computing_data_collection       'STOE SOFTWARE'
_computing_data_reduction        'STOE SOFTWARE'
_computing_molecular_graphics    POVRAY
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'STOE IPDS 1'
_diffrn_measurement_method       '1.5 deg phi 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  0.0890
_diffrn_reflns_av_sigmaI/netI    0.1412
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10976
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.5
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6167
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square pillar'
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.425
_refine_diff_density_min         -1.819
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0690
_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)+(0.0861P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1729
_reflns_number_gt                3769
_reflns_number_total             4939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911460b.txt
_cod_data_source_block           2
_cod_original_cell_volume        1322.5(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024134
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 0.37038(5) 0.13433(5) 0.49274(5) 0.02192(16) Uani 1 1 d .
Cl2 Cl 0.5126(2) 0.3046(2) 0.4093(3) 0.0354(6) Uani 1 1 d .
Cl3 Cl 0.1869(2) -0.0102(2) 0.5593(3) 0.0369(6) Uani 1 1 d .
Cl4 Cl 0.4139(3) -0.0949(2) 0.3639(2) 0.0383(6) Uani 1 1 d .
N6 N 0.4212(8) 0.2980(7) 0.7038(7) 0.0268(16) Uani 1 1 d .
N7 N 0.2110(8) 0.0770(7) 0.2847(8) 0.0288(17) Uani 1 1 d .
N9 N 0.2130(8) 0.2923(8) 0.4931(9) 0.0316(19) Uani 1 1 d .
C2 C 0.0453(8) 0.4568(9) 0.4995(9) 0.0255(19) Uani 1 1 d .
C3 C 0.0056(10) 0.3299(10) 0.4986(12) 0.038(3) Uani 1 1 d .
H3 H -0.0807 0.2954 0.4997 0.046 Uiso 1 1 calc R
C4 C 0.0924(10) 0.2522(10) 0.4962(12) 0.038(3) Uani 1 1 d .
H4 H 0.0629 0.1653 0.4969 0.046 Uiso 1 1 calc R
C5 C 0.2489(9) 0.4123(9) 0.4901(11) 0.036(3) Uani 1 1 d .
H5 H 0.3347 0.4432 0.4857 0.043 Uiso 1 1 calc R
C6 C 0.1700(9) 0.4963(10) 0.4929(12) 0.040(3) Uani 1 1 d .
H6 H 0.2023 0.5820 0.4902 0.047 Uiso 1 1 calc R
C7 C 0.3988(11) 0.2526(9) 0.7952(10) 0.034(2) Uani 1 1 d .
H7 H 0.3605 0.1634 0.7795 0.041 Uiso 1 1 calc R
C8 C 0.4847(9) 0.4567(9) 0.9383(9) 0.028(2) Uani 1 1 d .
C9 C 0.4281(11) 0.3275(10) 0.9109(10) 0.038(2) Uani 1 1 d .
H9 H 0.4092 0.2898 0.9724 0.045 Uiso 1 1 calc R
C10 C 0.0429(9) 0.0164(9) 0.0599(9) 0.027(2) Uani 1 1 d .
C11 C 0.1313(10) 0.1342(11) 0.1069(11) 0.037(2) Uani 1 1 d .
H11 H 0.1366 0.1965 0.0629 0.044 Uiso 1 1 calc R
C12 C 0.4742(11) 0.4225(11) 0.7289(10) 0.039(2) Uani 1 1 d .
H12 H 0.4928 0.4568 0.6654 0.047 Uiso 1 1 calc R
C13 C 0.2484(11) -0.2299(12) -0.0504(11) 0.040(3) Uani 1 1 d .
C14 C 0.3316(11) -0.1336(11) 0.0453(12) 0.044(3) Uani 1 1 d .
H14 H 0.3662 -0.1530 0.1166 0.053 Uiso 1 1 calc R
C15 C 0.5038(13) 0.5049(11) 0.8411(11) 0.045(3) Uani 1 1 d .
H15 H 0.5372 0.5945 0.8532 0.054 Uiso 1 1 calc R
C16 C 0.0444(11) -0.0699(11) 0.1283(11) 0.042(3) Uani 1 1 d .
H16 H -0.0133 -0.1526 0.0998 0.050 Uiso 1 1 calc R
C17 C 0.1294(11) -0.0364(11) 0.2377(11) 0.041(3) Uani 1 1 d .
H17 H 0.1290 -0.0986 0.2818 0.049 Uiso 1 1 calc R
C18 C 0.2124(10) 0.1605(11) 0.2187(10) 0.039(2) Uani 1 1 d .
H18 H 0.2719 0.2421 0.2496 0.046 Uiso 1 1 calc R
N19 N 0.1295(10) -0.6167(11) -0.0307(13) 0.058(3) Uani 1 1 d .
N2 N 0.3192(13) 0.0300(12) -0.0601(12) 0.060(3) Uani 1 1 d .
C1 C 0.2059(11) -0.3601(12) -0.0436(11) 0.043(3) Uani 1 1 d .
C20 C 0.1982(12) -0.3884(13) 0.0633(12) 0.046(3) Uani 1 1 d .
H20 H 0.2190 -0.3205 0.1349 0.056 Uiso 1 1 calc R
C21 C 0.3631(13) -0.0088(13) 0.0345(13) 0.052(3) Uani 1 1 d .
H21 H 0.4210 0.0545 0.1005 0.062 Uiso 1 1 calc R
C22 C 0.1748(12) -0.4660(13) -0.1453(14) 0.052(3) Uani 1 1 d .
H22 H 0.1781 -0.4525 -0.2213 0.063 Uiso 1 1 calc R
C23 C 0.1397(14) -0.5891(14) -0.1345(14) 0.057(3) Uani 1 1 d .
H23 H 0.1214 -0.6588 -0.2043 0.068 Uiso 1 1 calc R
C24 C 0.1605(13) -0.5141(16) 0.0667(15) 0.060(4) Uani 1 1 d .
H24 H 0.1560 -0.5298 0.1417 0.072 Uiso 1 1 calc R
C25 C 0.1980(14) -0.1893(16) -0.1495(14) 0.059(4) Uani 1 1 d .
H25 H 0.1365 -0.2491 -0.2153 0.071 Uiso 1 1 calc R
C26 C 0.2376(16) -0.0635(17) -0.1511(15) 0.065(4) Uani 1 1 d .
H26 H 0.2051 -0.0409 -0.2213 0.078 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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_3
N6 Pr1 N7 139.3(2) .
N6 Pr1 Cl3 87.96(19) .
N7 Pr1 Cl3 86.9(2) .
N6 Pr1 N9 70.3(3) .
N7 Pr1 N9 69.0(3) .
Cl3 Pr1 N9 83.75(18) .
N6 Pr1 Cl2 91.83(18) .
N7 Pr1 Cl2 84.77(19) .
Cl3 Pr1 Cl2 166.96(7) .
N9 Pr1 Cl2 83.90(19) .
N6 Pr1 Cl4 144.35(17) .
N7 Pr1 Cl4 75.64(18) .
Cl3 Pr1 Cl4 87.59(9) .
N9 Pr1 Cl4 143.9(2) .
Cl2 Pr1 Cl4 100.01(9) .
N6 Pr1 Cl4 71.48(18) 2_656
N7 Pr1 Cl4 149.09(18) 2_656
Cl3 Pr1 Cl4 99.12(9) 2_656
N9 Pr1 Cl4 141.6(2) 2_656
Cl2 Pr1 Cl4 93.16(9) 2_656
Cl4 Pr1 Cl4 74.37(9) 2_656
Pr1 Cl4 Pr1 105.63(9) 2_656
C12 N6 C7 116.6(9) .
C12 N6 Pr1 125.1(7) .
C7 N6 Pr1 118.2(6) .
C17 N7 C18 116.6(9) .
C17 N7 Pr1 122.3(7) .
C18 N7 Pr1 121.0(6) .
C5 N9 C4 116.0(9) .
C5 N9 Pr1 123.3(6) .
C4 N9 Pr1 120.8(6) .
C3 C2 C6 115.9(9) .
C3 C2 C2 121.5(10) 2_566
C6 C2 C2 122.6(10) 2_566
C4 C3 C2 119.7(9) .
N9 C4 C3 123.8(10) .
N9 C5 C6 124.3(9) .
C5 C6 C2 120.3(9) .
N6 C7 C9 123.6(9) .
C9 C8 C15 115.7(10) .
C9 C8 C8 122.7(11) 2_667
C15 C8 C8 121.4(11) 2_667
C7 C9 C8 120.4(10) .
C11 C10 C16 116.3(9) .
C11 C10 C10 121.2(10) 2
C16 C10 C10 122.4(11) 2
C10 C11 C18 119.6(9) .
N6 C12 C15 123.8(10) .
C14 C13 C25 115.8(12) .
C14 C13 C1 122.2(11) .
C25 C13 C1 121.7(13) .
C13 C14 C21 118.9(12) .
C12 C15 C8 119.8(10) .
C10 C16 C17 120.2(10) .
N7 C17 C16 123.8(10) .
N7 C18 C11 123.3(10) .
C23 N19 C24 115.6(11) .
C21 N2 C26 114.7(12) .
C20 C1 C22 116.3(12) .
C20 C1 C13 122.1(12) .
C22 C1 C13 121.6(11) .
C24 C20 C1 120.4(14) .
N2 C21 C14 125.8(15) .
C23 C22 C1 119.9(13) .
N19 C23 C22 123.9(14) .
N19 C24 C20 123.8(13) .
C26 C25 C13 120.2(15) .
N2 C26 C25 124.5(13) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 N6 2.618(8) .
Pr1 N7 2.618(8) .
Pr1 Cl3 2.660(3) .
Pr1 N9 2.670(8) .
Pr1 Cl2 2.676(3) .
Pr1 Cl4 2.804(3) .
Pr1 Cl4 2.821(3) 2_656
Cl4 Pr1 2.821(3) 2_656
N6 C12 1.320(13) .
N6 C7 1.332(13) .
N7 C17 1.319(14) .
N7 C18 1.335(13) .
N9 C5 1.312(12) .
N9 C4 1.318(13) .
C2 C3 1.375(14) .
C2 C6 1.372(13) .
C2 C2 1.499(19) 2_566
C3 C4 1.394(14) .
C5 C6 1.379(15) .
C7 C9 1.372(16) .
C8 C9 1.372(13) .
C8 C15 1.403(15) .
C8 C8 1.49(2) 2_667
C10 C11 1.385(14) .
C10 C16 1.381(14) .
C10 C10 1.479(19) 2
C11 C18 1.391(15) .
C12 C15 1.369(17) .
C13 C14 1.396(19) .
C13 C25 1.409(17) .
C13 C1 1.442(17) .
C14 C21 1.389(17) .
C16 C17 1.380(16) .
N19 C23 1.348(19) .
N19 C24 1.36(2) .
N2 C21 1.333(18) .
N2 C26 1.35(2) .
C1 C20 1.383(17) .
C1 C22 1.407(19) .
C20 C24 1.376(19) .
C22 C23 1.375(19) .
C25 C26 1.37(2) .
