#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:27:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180506 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/75/7217553.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_7217553
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 Sm O7,3(Cl)'
_chemical_formula_sum            'C12 H22 Cl3 N4 O7 Sm'
_chemical_formula_weight         591.04
_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                 104.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.712(6)
_cell_length_b                   7.7286(15)
_cell_length_c                   19.559(4)
_cell_measurement_reflns_used    6267
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4747
_cell_measurement_theta_min      1.4626
_cell_volume                     4209.3(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10409
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    3.211
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.052
_refine_diff_density_max         3.550
_refine_diff_density_min         -1.829
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4779
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0747
_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)+(0.0704P)²+167.8820P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                4373
_reflns_number_total             4779
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7216639
_cod_data_source_file            c4ce00606b2.cif
_cod_data_source_block           1633
_cod_original_cell_volume        4209.1(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7217553
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
Sm1 Sm 0.608132(18) 0.27263(7) 0.20565(3) 0.02082(18) Uani 1 1 d .
Cl1 Cl 0.56301(9) 0.7883(3) 0.06722(13) 0.0278(5) Uani 1 1 d .
Cl2 Cl 0.56278(10) 0.7482(3) 0.31174(13) 0.0279(5) Uani 1 1 d .
Cl3 Cl 0.74961(9) 0.0358(4) 0.14830(14) 0.0309(6) Uani 1 1 d .
O1 O 0.5627(3) 0.2450(10) 0.0859(4) 0.0280(16) Uani 1 1 d .
O5 O 0.6986(2) 0.2701(11) 0.2393(4) 0.0293(17) Uani 1 1 d D
H15A H 0.714(4) 0.252(16) 0.208(5) 0.035 Uiso 1 1 d D
H15B H 0.709(4) 0.306(17) 0.281(3) 0.035 Uiso 1 1 d D
O3 O 0.5466(3) 0.5056(9) 0.1741(4) 0.0239(15) Uani 1 1 d D
H13B H 0.550(4) 0.572(13) 0.141(4) 0.029 Uiso 1 1 d D
H13A H 0.540(4) 0.549(15) 0.210(4) 0.029 Uiso 1 1 d D
O2 O 0.5621(3) 0.3078(11) 0.2902(4) 0.0301(17) Uani 1 1 d .
O6 O 0.5504(3) 0.0367(10) 0.1941(4) 0.0283(16) Uani 1 1 d D
H16A H 0.552(5) -0.040(12) 0.225(5) 0.034 Uiso 1 1 d D
H16B H 0.547(5) -0.012(15) 0.155(3) 0.034 Uiso 1 1 d D
N3 N 0.6404(3) 0.4367(12) 0.1072(5) 0.0258(18) Uani 1 1 d .
O7 O 0.6420(3) 0.0212(12) 0.1568(5) 0.0370(19) Uani 1 1 d D
H17B H 0.651(5) -0.003(19) 0.120(4) 0.044 Uiso 1 1 d D
H17A H 0.6716(12) 0.031(19) 0.174(7) 0.044 Uiso 1 1 d D
N1 N 0.6368(3) 0.1036(12) 0.3245(5) 0.0273(19) Uani 1 1 d .
O4 O 0.6408(3) 0.5279(11) 0.2740(5) 0.0365(19) Uani 1 1 d D
H14B H 0.624(4) 0.588(15) 0.296(7) 0.044 Uiso 1 1 d D
H14A H 0.667(3) 0.559(18) 0.302(6) 0.044 Uiso 1 1 d D
N4 N 0.5522(4) 0.2408(15) -0.0321(5) 0.035(2) Uani 1 1 d D
H24B H 0.563(5) 0.251(17) -0.071(5) 0.042 Uiso 1 1 d D
H24A H 0.526(3) 0.183(16) -0.028(7) 0.042 Uiso 1 1 d D
N2 N 0.5448(3) 0.2905(13) 0.3960(5) 0.029(2) Uani 1 1 d D
H22A H 0.535(3) 0.401(6) 0.387(4) 0.035 Uiso 1 1 d D
H22B H 0.549(3) 0.244(10) 0.440(3) 0.035 Uiso 1 1 d D
C12 C 0.5761(4) 0.2847(14) 0.0324(5) 0.023(2) Uani 1 1 d .
C6 C 0.5714(4) 0.2538(14) 0.3516(5) 0.027(2) Uani 1 1 d D
C1 C 0.6143(3) 0.1382(13) 0.3759(5) 0.023(2) Uani 1 1 d .
C7 C 0.6209(4) 0.3924(13) 0.0403(5) 0.025(2) Uani 1 1 d .
C2 C 0.6301(4) 0.0734(14) 0.4438(5) 0.026(2) Uani 1 1 d .
H2 H 0.6136 0.1015 0.4790 0.031 Uiso 1 1 calc R
C8 C 0.6401(4) 0.4456(15) -0.0150(5) 0.028(2) Uani 1 1 d .
H8 H 0.6258 0.4086 -0.0617 0.033 Uiso 1 1 calc R
C5 C 0.6742(4) -0.0063(14) 0.3399(6) 0.028(2) Uani 1 1 d .
H5 H 0.6894 -0.0367 0.3036 0.034 Uiso 1 1 calc R
C9 C 0.6794(4) 0.5503(15) -0.0025(7) 0.035(3) Uani 1 1 d .
H9 H 0.6934 0.5839 -0.0397 0.042 Uiso 1 1 calc R
C4 C 0.6916(4) -0.0779(14) 0.4067(5) 0.026(2) Uani 1 1 d .
H4 H 0.7179 -0.1563 0.4154 0.031 Uiso 1 1 calc R
C11 C 0.6780(4) 0.5443(15) 0.1189(6) 0.031(2) Uani 1 1 d .
H11 H 0.6916 0.5801 0.1661 0.037 Uiso 1 1 calc R
C10 C 0.6985(4) 0.6069(15) 0.0661(6) 0.031(2) Uani 1 1 d .
H10 H 0.7246 0.6858 0.0766 0.038 Uiso 1 1 calc R
C3 C 0.6702(4) -0.0328(15) 0.4597(6) 0.033(2) Uani 1 1 d .
H3 H 0.6826 -0.0737 0.5064 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'
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
O2 Sm1 O1 115.4(3)
O2 Sm1 O6 70.6(3)
O1 Sm1 O6 69.3(3)
O2 Sm1 O4 74.3(3)
O1 Sm1 O4 130.8(3)
O6 Sm1 O4 144.8(3)
O2 Sm1 O7 134.4(3)
O1 Sm1 O7 73.9(3)
O6 Sm1 O7 72.4(3)
O4 Sm1 O7 135.6(3)
O2 Sm1 O3 66.9(2)
O1 Sm1 O3 68.8(2)
O6 Sm1 O3 95.3(3)
O4 Sm1 O3 72.9(3)
O7 Sm1 O3 142.7(3)
O2 Sm1 O5 122.2(3)
O1 Sm1 O5 122.4(3)
O6 Sm1 O5 130.8(3)
O4 Sm1 O5 68.2(3)
O7 Sm1 O5 67.5(3)
O3 Sm1 O5 133.9(3)
O2 Sm1 N1 63.0(3)
O1 Sm1 N1 143.3(3)
O6 Sm1 N1 76.6(3)
O4 Sm1 N1 85.5(3)
O7 Sm1 N1 83.3(3)
O3 Sm1 N1 129.1(2)
O5 Sm1 N1 71.5(3)
O2 Sm1 N3 143.5(3)
O1 Sm1 N3 62.4(3)
O6 Sm1 N3 129.8(3)
O4 Sm1 N3 81.7(3)
O7 Sm1 N3 81.7(3)
O3 Sm1 N3 80.0(2)
O5 Sm1 N3 70.9(3)
N1 Sm1 N3 142.5(3)
C12 O1 Sm1 126.7(7)
C6 O2 Sm1 127.8(7)
C7 N3 C11 117.1(9)
C7 N3 Sm1 116.8(7)
C11 N3 Sm1 125.6(7)
C5 N1 C1 117.4(9)
C5 N1 Sm1 125.1(7)
C1 N1 Sm1 117.4(7)
O1 C12 N4 123.0(10)
O1 C12 C7 118.8(9)
N4 C12 C7 118.1(9)
O2 C6 N2 123.0(11)
O2 C6 C1 118.3(10)
N2 C6 C1 118.7(9)
N1 C1 C2 122.6(10)
N1 C1 C6 112.7(9)
C2 C1 C6 124.6(9)
N3 C7 C8 122.3(10)
N3 C7 C12 112.7(9)
C8 C7 C12 124.9(10)
C3 C2 C1 119.1(10)
C9 C8 C7 120.2(10)
N1 C5 C4 123.0(10)
C8 C9 C10 118.4(10)
C3 C4 C5 118.8(10)
N3 C11 C10 123.8(10)
C9 C10 C11 117.9(11)
C4 C3 C2 118.8(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sm1 O2 2.370(7)
Sm1 O1 2.396(7)
Sm1 O6 2.437(8)
Sm1 O4 2.439(8)
Sm1 O7 2.468(8)
Sm1 O3 2.492(7)
Sm1 O5 2.520(7)
Sm1 N1 2.618(9)
Sm1 N3 2.654(9)
O1 C12 1.239(12)
O2 C6 1.237(12)
N3 C7 1.335(13)
N3 C11 1.339(14)
N1 C5 1.344(14)
N1 C1 1.347(13)
N4 C12 1.324(14)
N2 C6 1.319(14)
C12 C7 1.507(15)
C6 C1 1.503(15)
C1 C2 1.388(14)
C7 C8 1.392(14)
C2 C3 1.386(15)
C8 C9 1.361(16)
C5 C4 1.395(14)
C9 C10 1.389(17)
C4 C3 1.373(16)
C11 C10 1.394(15)
