#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:27:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180506 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/75/7217550.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_7217550
loop_
_publ_author_name
'Xue, Jun-Hui'
'Hua, Xiao-Hui'
'Yang, Li-Min'
'Li, Wei-Hong'
'Xu, Yi-Zhuang'
'Zhao, Guo-Zhong'
'Zhang, Gao-Hui'
'Liu, Ke-Xin'
'Chen, Jia-Er'
'Wu, Jin-Guang'
_publ_section_title
;
 The coordination of lanthanide ions with picolinamide. The influence of
 different anions
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              7711
_journal_paper_doi               10.1039/C4CE00606B
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C12 H22 N4 La O7,3(Cl)'
_chemical_formula_sum            'C12 H22 Cl3 La N4 O7'
_chemical_formula_weight         579.60
_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                 104.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.898(6)
_cell_length_b                   7.7600(16)
_cell_length_c                   19.778(4)
_cell_measurement_reflns_used    7210
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4851
_cell_measurement_theta_min      1.4550
_cell_volume                     4296.0(16)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics
;
Mercury: visualization and analysis of crystal structures, C. F. Macrae,
P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15489
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0537
_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)+(0.0400P)²+18.2173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                4444
_reflns_number_total             4909
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7216636
_cod_data_source_file            c4ce00606b2.cif
_cod_data_source_block           mx1358
_cod_original_cell_volume        4296.1(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7217550
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
La1 La 0.108158(11) 0.77250(4) 0.206269(16) 0.02089(11) Uani 1 1 d .
Cl1 Cl 0.06280(5) 0.2867(2) 0.06827(7) 0.0276(3) Uani 1 1 d .
Cl2 Cl 0.06225(5) 0.24776(19) 0.31166(7) 0.0287(3) Uani 1 1 d .
Cl3 Cl 0.24949(5) 0.5397(2) 0.14832(8) 0.0325(3) Uani 1 1 d .
O2 O 0.06261(14) 0.7516(5) 0.0830(2) 0.0273(9) Uani 1 1 d .
O6 O 0.20021(14) 0.7681(5) 0.2411(2) 0.0301(10) Uani 1 1 d .
H6A H 0.2187 0.7264 0.2186 0.036 Uiso 1 1 d R
H6B H 0.2197 0.8337 0.2677 0.036 Uiso 1 1 d R
O3 O 0.04456(13) 1.0082(5) 0.17436(19) 0.0248(9) Uani 1 1 d .
H3A H 0.0425 1.0787 0.2057 0.030 Uiso 1 1 d R
H3B H 0.0394 1.0456 0.1333 0.030 Uiso 1 1 d R
O1 O 0.06183(15) 0.8031(6) 0.2939(2) 0.0291(9) Uani 1 1 d .
O5 O 0.04955(14) 0.5279(5) 0.1930(2) 0.0293(9) Uani 1 1 d .
H5A H 0.0407 0.4752 0.1548 0.035 Uiso 1 1 d R
H5B H 0.0506 0.4506 0.2230 0.035 Uiso 1 1 d R
O7 O 0.14399(15) 0.5121(6) 0.1581(2) 0.0417(12) Uani 1 1 d .
H7A H 0.1273 0.4417 0.1301 0.050 Uiso 1 1 d R
H7B H 0.1635 0.5180 0.1329 0.050 Uiso 1 1 d R
O4 O 0.14202(15) 1.0384(6) 0.2751(2) 0.0417(12) Uani 1 1 d .
H4A H 0.1218 1.0971 0.2891 0.050 Uiso 1 1 d R
H4B H 0.1691 1.0485 0.3029 0.050 Uiso 1 1 d R
N3 N 0.14133(17) 0.9395(7) 0.1044(2) 0.0266(11) Uani 1 1 d .
N1 N 0.13732(16) 0.6025(6) 0.3297(2) 0.0243(10) Uani 1 1 d .
N4 N 0.05181(19) 0.7471(7) -0.0328(3) 0.0354(13) Uani 1 1 d .
H4C H 0.0251 0.6883 -0.0384 0.043 Uiso 1 1 calc R
H4D H 0.0623 0.7766 -0.0693 0.043 Uiso 1 1 calc R
N2 N 0.04457(18) 0.7874(7) 0.3982(3) 0.0300(12) Uani 1 1 d .
H2D H 0.0191 0.8528 0.3839 0.036 Uiso 1 1 calc R
H2C H 0.0521 0.7476 0.4412 0.036 Uiso 1 1 calc R
C6 C 0.0715(2) 0.7490(7) 0.3550(3) 0.0247(12) Uani 1 1 d .
C1 C 0.11420(19) 0.6352(7) 0.3798(3) 0.0221(12) Uani 1 1 d .
C12 C 0.0761(2) 0.7907(8) 0.0300(3) 0.0264(13) Uani 1 1 d .
C7 C 0.1209(2) 0.8953(8) 0.0380(3) 0.0260(12) Uani 1 1 d .
C11 C 0.1793(2) 1.0426(8) 0.1163(3) 0.0319(14) Uani 1 1 d .
H11 H 0.1938 1.0748 0.1632 0.038 Uiso 1 1 calc R
C8 C 0.1390(2) 0.9468(8) -0.0174(3) 0.0284(13) Uani 1 1 d .
H8 H 0.1242 0.9111 -0.0637 0.034 Uiso 1 1 calc R
C5 C 0.1744(2) 0.4935(8) 0.3455(3) 0.0307(14) Uani 1 1 d .
H5 H 0.1899 0.4642 0.3100 0.037 Uiso 1 1 calc R
C4 C 0.1910(2) 0.4217(8) 0.4108(3) 0.0300(13) Uani 1 1 d .
H4 H 0.2174 0.3446 0.4197 0.036 Uiso 1 1 calc R
C2 C 0.1291(2) 0.5707(8) 0.4468(3) 0.0288(13) Uani 1 1 d .
H2 H 0.1125 0.5993 0.4812 0.035 Uiso 1 1 calc R
C9 C 0.1791(2) 1.0516(9) -0.0041(3) 0.0358(15) Uani 1 1 d .
H9 H 0.1929 1.0858 -0.0409 0.043 Uiso 1 1 calc R
C3 C 0.1690(2) 0.4630(8) 0.4632(3) 0.0315(14) Uani 1 1 d .
H3 H 0.1806 0.4191 0.5091 0.038 Uiso 1 1 calc R
C10 C 0.1989(2) 1.1055(8) 0.0636(3) 0.0336(14) Uani 1 1 d .
H10 H 0.2250 1.1834 0.0739 0.040 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'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 La1 O2 116.98(13)
O1 La1 O5 71.04(14)
O2 La1 O5 70.57(13)
O1 La1 O4 75.33(15)
O2 La1 O4 128.60(15)
O5 La1 O4 146.33(13)
O1 La1 O3 67.68(13)
O2 La1 O3 68.26(13)
O5 La1 O3 95.16(14)
O4 La1 O3 73.02(13)
O1 La1 O7 133.04(15)
O2 La1 O7 75.31(14)
O5 La1 O7 71.91(13)
O4 La1 O7 134.88(14)
O3 La1 O7 143.57(14)
O1 La1 O6 121.39(14)
O2 La1 O6 121.62(13)
O5 La1 O6 129.94(13)
O4 La1 O6 68.37(13)
O3 La1 O6 134.91(13)
O7 La1 O6 66.62(13)
O1 La1 N1 60.89(13)
O2 La1 N1 145.55(14)
O5 La1 N1 77.18(14)
O4 La1 N1 85.43(15)
O3 La1 N1 127.73(12)
O7 La1 N1 83.56(15)
O6 La1 N1 71.59(14)
O1 La1 N3 145.15(14)
O2 La1 N3 60.47(14)
O5 La1 N3 128.71(14)
O4 La1 N3 81.47(15)
O3 La1 N3 80.95(13)
O7 La1 N3 81.53(15)
O6 La1 N3 71.26(14)
N1 La1 N3 142.85(14)
C12 O2 La1 127.9(4)
C6 O1 La1 128.6(4)
C11 N3 C7 118.0(5)
C11 N3 La1 125.0(4)
C7 N3 La1 116.4(4)
C5 N1 C1 117.5(5)
C5 N1 La1 124.5(4)
C1 N1 La1 117.9(4)
O1 C6 N2 121.6(6)
O1 C6 C1 119.0(5)
N2 C6 C1 119.4(5)
N1 C1 C2 122.9(5)
N1 C1 C6 112.9(5)
C2 C1 C6 124.2(5)
O2 C12 N4 122.1(6)
O2 C12 C7 119.0(5)
N4 C12 C7 118.9(5)
N3 C7 C8 122.6(6)
N3 C7 C12 113.5(5)
C8 C7 C12 123.9(5)
N3 C11 C10 123.3(6)
C9 C8 C7 118.8(6)
N1 C5 C4 123.1(5)
C5 C4 C3 119.4(6)
C1 C2 C3 118.8(5)
C10 C9 C8 119.0(6)
C4 C3 C2 118.3(6)
C9 C10 C11 118.2(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
La1 O1 2.451(4)
La1 O2 2.472(4)
La1 O5 2.513(4)
La1 O4 2.531(4)
La1 O3 2.558(4)
La1 O7 2.560(4)
La1 O6 2.577(4)
La1 N1 2.718(5)
La1 N3 2.759(5)
O2 C12 1.242(7)
O1 C6 1.243(7)
N3 C11 1.331(8)
N3 C7 1.344(7)
N1 C5 1.339(7)
N1 C1 1.349(6)
N4 C12 1.310(7)
N2 C6 1.324(7)
C6 C1 1.498(8)
C1 C2 1.383(8)
C12 C7 1.503(8)
C7 C8 1.387(7)
C11 C10 1.392(8)
C8 C9 1.387(9)
C5 C4 1.380(8)
C4 C3 1.381(8)
C2 C3 1.395(8)
C9 C10 1.384(9)
