#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:59:31 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179946 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/41/7024133.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_7024133
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[Sm2Cl6(C10H8N2)3](C10H8N2)2
_chemical_formula_sum            'C25 H20 Cl3 N5 Sm'
_chemical_formula_weight         647.16
_chemical_name_common
;2D-(Hexakis-chloro-tris-(4,4-bipyridino)-di-samarium(iii))-di-
4,4-bipridine
;
_chemical_name_systematic
;
2D-[Hexakis-chloro-tris-(4,4-bipyridino)-di-samarium(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
_cell_angle_alpha                101.78(3)
_cell_angle_beta                 103.71(3)
_cell_angle_gamma                100.21(3)
_cell_formula_units_Z            2
_cell_length_a                   10.963(2)
_cell_length_b                   10.985(2)
_cell_length_c                   11.960(2)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      53.96
_cell_measurement_theta_min      3.62
_cell_volume                     1330.7(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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS 1'
_diffrn_measurement_method       '1 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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20585
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    2.530
_exptl_absorpt_correction_T_max  0.7561
_exptl_absorpt_correction_T_min  0.6182
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square pillar'
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.031
_refine_diff_density_min         -2.786
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0387P)²+1.4052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                5504
_reflns_number_total             5700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911460b.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024133
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
Sm1 Sm 0.63329(3) 0.87022(3) 0.99536(3) 0.02072(12) Uani 1 1 d .
Cl4 Cl 0.48610(18) 0.69177(19) 1.05570(19) 0.0375(4) Uani 1 1 d .
N3 N 0.7948(6) 0.9216(6) 1.2043(5) 0.0291(13) Uani 1 1 d .
N1 N 0.5776(6) 0.7132(6) 0.7883(5) 0.0304(14) Uani 1 1 d .
Cl1 Cl 0.58846(18) 1.0816(2) 1.13804(15) 0.0369(5) Uani 1 1 d .
Cl2 Cl 0.80578(18) 1.01332(19) 0.92455(19) 0.0370(4) Uani 1 1 d .
N2 N 0.7884(6) 0.7132(6) 0.9958(6) 0.0297(13) Uani 1 1 d .
C13 C 0.9570(6) 0.9833(7) 1.4382(6) 0.044(2) Uani 1 1 d .
C3 C 0.5161(7) 0.5437(7) 0.5612(6) 0.046(2) Uani 1 1 d .
C6 C 0.9121(8) 0.7482(8) 0.9926(9) 0.044(2) Uani 1 1 d .
H6 H 0.9429 0.8332 0.9885 0.053 Uiso 1 1 calc R
C10 C 0.7501(8) 0.5919(8) 0.9981(9) 0.040(2) Uani 1 1 d .
H10 H 0.6635 0.5625 0.9989 0.048 Uiso 1 1 calc R
C7 C 0.9956(8) 0.6693(8) 0.9948(10) 0.046(2) Uani 1 1 d .
H7 H 1.0816 0.7007 0.9934 0.055 Uiso 1 1 calc R
C5 C 0.4635(10) 0.6299(10) 0.7387(8) 0.050(2) Uani 1 1 d .
H5 H 0.4016 0.6294 0.7825 0.060 Uiso 1 1 calc R
C15 C 0.7531(9) 0.8946(10) 1.2900(8) 0.050(2) Uani 1 1 d .
H15 H 0.6650 0.8513 1.2720 0.060 Uiso 1 1 calc R
C1 C 0.6566(10) 0.7159(9) 0.7194(8) 0.052(3) Uani 1 1 d .
H1 H 0.7353 0.7799 0.7482 0.063 Uiso 1 1 calc R
C14 C 0.8285(9) 0.9246(11) 1.4076(8) 0.052(3) Uani 1 1 d .
H14 H 0.7906 0.9043 1.4672 0.062 Uiso 1 1 calc R
C4 C 0.4290(10) 0.5440(10) 0.6277(8) 0.053(3) Uani 1 1 d .
H4 H 0.3464 0.4861 0.5977 0.063 Uiso 1 1 calc R
C8 C 0.9558(7) 0.5447(7) 0.9991(6) 0.042(2) Uani 1 1 d .
C9 C 0.8286(8) 0.5056(8) 0.9995(9) 0.042(2) Uani 1 1 d .
H9 H 0.7953 0.4201 1.0006 0.050 Uiso 1 1 calc R
N4 N 1.1175(10) 1.3721(10) 1.5215(11) 0.076(3) Uani 1 1 d .
C21 C 0.7284(10) 1.2516(10) 1.5495(8) 0.049(2) Uani 1 1 d .
C12 C 1.0036(10) 1.0071(11) 1.3444(9) 0.057(3) Uani 1 1 d .
H12 H 1.0925 1.0459 1.3595 0.068 Uiso 1 1 calc R
C22 C 0.6337(10) 1.1653(10) 1.4549(9) 0.054(3) Uani 1 1 d .
H22 H 0.6533 1.1268 1.3847 0.065 Uiso 1 1 calc R
C2 C 0.6327(10) 0.6331(9) 0.6102(8) 0.052(2) Uani 1 1 d .
H2 H 0.6961 0.6372 0.5682 0.062 Uiso 1 1 calc R
C18 C 0.8579(11) 1.2954(10) 1.5426(9) 0.055(3) Uani 1 1 d .
C11 C 0.9232(9) 0.9756(11) 1.2301(8) 0.055(3) Uani 1 1 d .
H11 H 0.9582 0.9919 1.1677 0.066 Uiso 1 1 calc R
C23 C 0.5063(12) 1.1358(12) 1.4660(11) 0.066(3) Uani 1 1 d .
H23 H 0.4418 1.0777 1.3998 0.079 Uiso 1 1 calc R
N5 N 0.4688(12) 1.1832(12) 1.5628(11) 0.083(3) Uani 1 1 d .
C17 C 0.8832(11) 1.2998(11) 1.4343(10) 0.060(3) Uani 1 1 d .
H17 H 0.8140 1.2782 1.3632 0.072 Uiso 1 1 calc R
C19 C 0.9654(12) 1.3270(11) 1.6441(11) 0.063(3) Uani 1 1 d .
H19 H 0.9547 1.3234 1.7200 0.076 Uiso 1 1 calc R
C25 C 0.6908(13) 1.3051(13) 1.6524(10) 0.067(3) Uani 1 1 d .
H25 H 0.7526 1.3659 1.7187 0.080 Uiso 1 1 calc R
C16 C 1.0108(13) 1.3362(12) 1.4313(13) 0.070(3) Uani 1 1 d .
H16 H 1.0225 1.3351 1.3549 0.084 Uiso 1 1 calc R
C20 C 1.0899(12) 1.3642(13) 1.6294(13) 0.074(3) Uani 1 1 d .
H20 H 1.1614 1.3858 1.6987 0.089 Uiso 1 1 calc R
C24 C 0.5631(14) 1.2676(15) 1.6545(12) 0.079(4) Uani 1 1 d .
H24 H 0.5410 1.3031 1.7242 0.095 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'
Sm Sm -0.1638 3.4418 '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
N1 Sm1 N3 139.7(2) . .
N1 Sm1 N2 69.4(2) . .
N3 Sm1 N2 70.3(2) . .
N1 Sm1 Cl4 87.54(16) . .
N3 Sm1 Cl4 88.43(15) . .
N2 Sm1 Cl4 84.17(15) . .
N1 Sm1 Cl2 86.10(15) . .
N3 Sm1 Cl2 90.27(15) . .
N2 Sm1 Cl2 84.69(15) . .
Cl4 Sm1 Cl2 168.56(6) . .
N1 Sm1 Cl1 74.71(15) . 2_677
N3 Sm1 Cl1 145.30(14) . 2_677
N2 Sm1 Cl1 143.68(14) . 2_677
Cl4 Sm1 Cl1 88.98(7) . 2_677
Cl2 Sm1 Cl1 98.48(7) . 2_677
N1 Sm1 Cl1 148.26(15) . .
N3 Sm1 Cl1 71.98(15) . .
N2 Sm1 Cl1 142.16(14) . .
Cl4 Sm1 Cl1 97.48(7) . .
Cl2 Sm1 Cl1 92.92(7) . .
Cl1 Sm1 Cl1 74.07(6) 2_677 .
C15 N3 C11 117.0(7) . .
C15 N3 Sm1 118.9(5) . .
C11 N3 Sm1 124.1(5) . .
C1 N1 C5 115.0(7) . .
C1 N1 Sm1 122.5(5) . .
C5 N1 Sm1 122.3(5) . .
Sm1 Cl1 Sm1 105.93(6) 2_677 .
C10 N2 C6 114.9(7) . .
C10 N2 Sm1 122.0(5) . .
C6 N2 Sm1 123.1(5) . .
C14 C13 C12 115.3(7) . .
C14 C13 C13 123.1(8) . 2_778
C12 C13 C13 121.6(8) . 2_778
C4 C3 C2 116.6(7) . .
C4 C3 C3 122.1(8) . 2_666
C2 C3 C3 121.2(8) . 2_666
N2 C6 C7 124.4(8) . .
N2 C10 C9 124.2(7) . .
C6 C7 C8 120.3(8) . .
N1 C5 C4 124.4(9) . .
N3 C15 C14 124.3(8) . .
N1 C1 C2 124.7(9) . .
C13 C14 C15 120.4(8) . .
C3 C4 C5 119.2(9) . .
C7 C8 C9 116.4(7) . .
C7 C8 C8 121.9(8) . 2_767
C9 C8 C8 121.7(8) . 2_767
C8 C9 C10 119.8(7) . .
C16 N4 C20 111.4(11) . .
C22 C21 C25 117.5(10) . .
C22 C21 C18 121.8(9) . .
C25 C21 C18 120.5(10) . .
C11 C12 C13 121.2(9) . .
C21 C22 C23 118.0(10) . .
C1 C2 C3 119.8(9) . .
C17 C18 C19 117.0(11) . .
C17 C18 C21 121.7(10) . .
C19 C18 C21 121.2(10) . .
N3 C11 C12 121.6(9) . .
N5 C23 C22 125.7(12) . .
C23 N5 C24 115.4(11) . .
C18 C17 C16 119.5(12) . .
C18 C19 C20 118.0(12) . .
C24 C25 C21 119.7(12) . .
N4 C16 C17 128.1(12) . .
N4 C20 C19 126.0(12) . .
N5 C24 C25 123.8(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm1 N1 2.578(6) .
Sm1 N3 2.583(6) .
Sm1 N2 2.628(6) .
Sm1 Cl4 2.641(2) .
Sm1 Cl2 2.648(2) .
Sm1 Cl1 2.774(2) 2_677
Sm1 Cl1 2.780(2) .
N3 C15 1.283(11) .
N3 C11 1.362(11) .
N1 C1 1.329(11) .
N1 C5 1.332(11) .
Cl1 Sm1 2.774(2) 2_677
N2 C10 1.333(10) .
N2 C6 1.355(10) .
C13 C14 1.368(11) .
C13 C12 1.390(12) .
C13 C13 1.486(13) 2_778
C3 C4 1.380(11) .
C3 C2 1.381(12) .
C3 C3 1.501(13) 2_666
C6 C7 1.367(12) .
C10 C9 1.389(11) .
C7 C8 1.377(11) .
C5 C4 1.386(12) .
C15 C14 1.390(12) .
C1 C2 1.368(12) .
C8 C9 1.385(10) .
C8 C8 1.497(14) 2_767
N4 C16 1.324(16) .
N4 C20 1.409(18) .
C21 C22 1.384(14) .
C21 C25 1.435(14) .
C21 C18 1.443(15) .
C12 C11 1.375(13) .
C22 C23 1.421(15) .
C18 C17 1.395(14) .
C18 C19 1.410(15) .
C23 N5 1.355(16) .
N5 C24 1.356(18) .
C17 C16 1.397(16) .
C19 C20 1.416(17) .
C25 C24 1.395(17) .
