#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:16:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180497 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/66/7216642.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_7216642
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 Pr O7,3(Br)'
_chemical_formula_sum            'C12 H22 Br3 N4 O7 Pr'
_chemical_formula_weight         714.98
_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                 103.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.485(6)
_cell_length_b                   7.8780(16)
_cell_length_c                   20.344(4)
_cell_measurement_reflns_used    7970
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4800
_cell_measurement_theta_min      1.4199
_cell_volume                     4597.1(17)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11646
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    7.371
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5249
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0646
_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)+(0.0840P)²+23.1609P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                4393
_reflns_number_total             5249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00606b2.cif
_cod_data_source_block           sa1756-a
_cod_depositor_comments
'Adding full bibliography for 7216635--7216642.cif.'
_cod_original_cell_volume        4597.1(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7216642
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
Pr1 Pr 0.107560(17) 0.22879(7) 0.20939(2) 0.03237(18) Uani 1 1 d D
Br1 Br 0.06139(4) 0.71662(14) 0.06702(5) 0.0456(3) Uani 1 1 d .
Br2 Br 0.05970(4) 0.74990(14) 0.31954(5) 0.0457(3) Uani 1 1 d .
Br3 Br 0.24931(4) 0.45772(17) 0.14416(6) 0.0527(3) Uani 1 1 d .
O1 O 0.0652(3) 0.2559(9) 0.0928(3) 0.0443(18) Uani 1 1 d .
O2 O 0.0623(2) 0.1942(9) 0.2944(3) 0.0401(16) Uani 1 1 d .
O3 O 0.0457(2) 0.0022(9) 0.1782(3) 0.0436(16) Uani 1 1 d .
H3A H 0.0493 -0.0563 0.1452 0.052 Uiso 1 1 d R
H3B H 0.0332 -0.0312 0.2090 0.052 Uiso 1 1 d R
O4 O 0.1970(3) 0.2315(9) 0.2417(4) 0.0488(19) Uani 1 1 d D
H4B H 0.2134 0.2021 0.2795 0.059 Uiso 1 1 d RD
H4A H 0.2147 0.2587 0.2165 0.059 Uiso 1 1 d RD
N3 N 0.1364(3) 0.3925(10) 0.3289(4) 0.0357(17) Uani 1 1 d .
N1 N 0.1409(3) 0.0681(11) 0.1117(4) 0.0412(19) Uani 1 1 d .
O5 O 0.0494(3) 0.4629(10) 0.1978(3) 0.0501(19) Uani 1 1 d D
H5A H 0.0323 0.4955 0.1610 0.060 Uiso 1 1 d RD
H5B H 0.0472 0.5312 0.2286 0.060 Uiso 1 1 d RD
O7 O 0.1419(3) 0.4846(10) 0.1644(5) 0.066(2) Uani 1 1 d D
H7B H 0.1651 0.4800 0.1471 0.079 Uiso 1 1 d RD
H7A H 0.1262 0.5711 0.1493 0.079 Uiso 1 1 d RD
O6 O 0.1394(3) -0.0295(10) 0.2740(4) 0.057(2) Uani 1 1 d D
H6B H 0.1603 -0.0139 0.3094 0.069 Uiso 1 1 d RD
H6A H 0.1198 -0.0980 0.2829 0.069 Uiso 1 1 d RD
C6 C 0.0789(4) 0.2178(13) 0.0402(4) 0.039(2) Uani 1 1 d .
C11 C 0.1726(4) 0.4981(14) 0.3428(6) 0.049(3) Uani 1 1 d .
H11 H 0.1878 0.5287 0.3081 0.059 Uiso 1 1 calc R
C7 C 0.1146(3) 0.3512(12) 0.3771(5) 0.037(2) Uani 1 1 d .
C12 C 0.0721(3) 0.2453(12) 0.3535(5) 0.037(2) Uani 1 1 d .
C5 C 0.1781(4) -0.0376(14) 0.1223(5) 0.051(3) Uani 1 1 d .
H5 H 0.1915 -0.0742 0.1671 0.061 Uiso 1 1 calc R
C1 C 0.1217(4) 0.1145(13) 0.0462(4) 0.038(2) Uani 1 1 d .
N2 N 0.0558(4) 0.2661(13) -0.0199(4) 0.057(3) Uani 1 1 d .
H2A H 0.0302 0.3264 -0.0242 0.068 Uiso 1 1 calc R
H2B H 0.0659 0.2382 -0.0558 0.068 Uiso 1 1 calc R
N4 N 0.0452(3) 0.2058(13) 0.3936(4) 0.051(2) Uani 1 1 d .
H4C H 0.0202 0.1432 0.3786 0.061 Uiso 1 1 calc R
H4D H 0.0519 0.2418 0.4357 0.061 Uiso 1 1 calc R
C10 C 0.1885(4) 0.5645(14) 0.4076(6) 0.050(3) Uani 1 1 d .
H10 H 0.2135 0.6433 0.4166 0.060 Uiso 1 1 calc R
C9 C 0.1680(4) 0.5161(14) 0.4576(5) 0.046(2) Uani 1 1 d .
H9 H 0.1801 0.5539 0.5026 0.056 Uiso 1 1 calc R
C8 C 0.1298(4) 0.4124(14) 0.4431(5) 0.045(2) Uani 1 1 d .
H8 H 0.1139 0.3826 0.4771 0.054 Uiso 1 1 calc R
C3 C 0.1787(4) -0.0416(16) 0.0052(6) 0.056(3) Uani 1 1 d .
H3 H 0.1919 -0.0771 -0.0309 0.067 Uiso 1 1 calc R
C2 C 0.1404(4) 0.0648(15) -0.0063(6) 0.051(3) Uani 1 1 d .
H2 H 0.1271 0.1036 -0.0508 0.062 Uiso 1 1 calc R
C4 C 0.1972(4) -0.0946(16) 0.0699(6) 0.056(3) Uani 1 1 d .
H4 H 0.2231 -0.1701 0.0790 0.067 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'
Br Br -0.2901 2.4595 '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
O1 Pr1 O2 117.6(2)
O1 Pr1 O6 129.5(3)
O2 Pr1 O6 74.6(3)
O1 Pr1 O5 69.8(2)
O2 Pr1 O5 70.8(2)
O6 Pr1 O5 145.4(3)
O1 Pr1 O7 74.5(3)
O2 Pr1 O7 132.9(3)
O6 Pr1 O7 135.4(2)
O5 Pr1 O7 72.5(3)
O1 Pr1 O3 68.8(2)
O2 Pr1 O3 67.4(2)
O6 Pr1 O3 73.5(2)
O5 Pr1 O3 93.4(3)
O7 Pr1 O3 143.3(3)
O1 Pr1 O4 121.1(3)
O2 Pr1 O4 121.3(2)
O6 Pr1 O4 68.4(2)
O5 Pr1 O4 131.4(2)
O7 Pr1 O4 67.1(2)
O3 Pr1 O4 135.2(2)
O1 Pr1 N3 145.2(2)
O2 Pr1 N3 61.6(2)
O6 Pr1 N3 85.0(3)
O5 Pr1 N3 78.4(2)
O7 Pr1 N3 82.9(3)
O3 Pr1 N3 128.3(2)
O4 Pr1 N3 71.1(2)
O1 Pr1 N1 61.2(2)
O2 Pr1 N1 144.8(2)
O6 Pr1 N1 81.4(3)
O5 Pr1 N1 129.1(2)
O7 Pr1 N1 82.1(3)
O3 Pr1 N1 81.4(2)
O4 Pr1 N1 70.6(2)
N3 Pr1 N1 141.7(2)
C6 O1 Pr1 128.0(7)
C12 O2 Pr1 127.7(6)
C11 N3 C7 119.7(8)
C11 N3 Pr1 123.9(7)
C7 N3 Pr1 116.1(6)
C5 N1 C1 117.2(9)
C5 N1 Pr1 125.8(7)
C1 N1 Pr1 116.6(6)
O1 C6 N2 121.5(10)
O1 C6 C1 119.5(8)
N2 C6 C1 119.0(9)
N3 C11 C10 120.8(10)
N3 C7 C8 121.4(9)
N3 C7 C12 114.3(8)
C8 C7 C12 124.2(9)
O2 C12 N4 119.5(9)
O2 C12 C7 119.1(9)
N4 C12 C7 121.4(9)
N1 C5 C4 122.2(10)
C2 C1 N1 122.1(10)
C2 C1 C6 125.6(9)
N1 C1 C6 112.3(8)
C9 C10 C11 119.7(10)
C10 C9 C8 119.6(9)
C9 C8 C7 118.5(10)
C4 C3 C2 118.5(11)
C1 C2 C3 120.2(11)
C3 C4 C5 119.7(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pr1 O1 2.421(7)
Pr1 O2 2.432(7)
Pr1 O6 2.486(7)
Pr1 O5 2.492(7)
Pr1 O7 2.520(8)
Pr1 O3 2.525(7)
Pr1 O4 2.566(7)
Pr1 N3 2.709(7)
Pr1 N1 2.725(8)
O1 C6 1.265(12)
O2 C12 1.237(12)
N3 C11 1.332(13)
N3 C7 1.332(12)
N1 C5 1.353(13)
N1 C1 1.370(12)
C6 N2 1.309(13)
C6 C1 1.483(14)
C11 C10 1.394(15)
C7 C8 1.398(14)
C7 C12 1.490(14)
C12 N4 1.302(13)
C5 C4 1.392(15)
C1 C2 1.368(14)
C10 C9 1.352(16)
C9 C8 1.368(15)
C3 C4 1.368(17)
C3 C2 1.381(16)
