#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:18:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179446 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/43/4334354.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_4334354
loop_
_publ_author_name
'Sumi Ganguly'
'Pradip Pachfule'
'Sukhen Bala'
'Arijit Goswami'
'Sudeshna Bhattacharya'
'Raju Mondal'
_publ_section_title
;
 Azide-Functionalized Lanthanide-Based Metal-Organic Frameworks Showing
 Selective CO2 Gas Adsorption and Postsynthetic Cavity Expansion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3588
_journal_page_last               3590
_journal_paper_doi               10.1021/ic302823r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C16 H15 N6 O12 Pr'
_chemical_formula_weight         624.25
_chemical_name_systematic
; 
 ? 
;
_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                100.634(3)
_cell_angle_beta                 91.382(3)
_cell_angle_gamma                111.021(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5713(10)
_cell_length_b                   9.9024(10)
_cell_length_c                   12.3279(13)
_cell_measurement_reflns_used    11117
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.82
_cell_measurement_theta_min      2.25
_cell_volume                     1066.73(19)
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_collection       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w 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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14004
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.363
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.732484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.03 (Bruker, 2001), R(int)=0.0562 before correction'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       Block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0205
_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)+(0.0316P)²+0.6961P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                4505
_reflns_number_total             4723
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic302823r_si_004.cif
_cod_data_source_block           12ssg026_0m
_cod_database_code               4334354
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 0.792197(11) 0.050553(12) 0.016255(9) 0.01134(5) Uani 1 1 d .
O1A O 0.99495(17) 0.29795(18) 0.09682(14) 0.0196(3) Uani 1 1 d .
C1A C 1.2635(2) 0.3960(2) 0.11408(18) 0.0146(4) Uani 1 1 d .
O1 O 0.7261(2) 0.10472(19) 0.22048(14) 0.0217(4) Uani 1 1 d .
C1 C 0.7812(3) -0.0083(3) 0.36571(19) 0.0189(5) Uani 1 1 d .
N1A N 1.6587(2) 0.5022(2) 0.24514(17) 0.0212(4) Uani 1 1 d .
N1 N 0.6601(3) 0.1153(3) 0.64299(18) 0.0288(5) Uani 1 1 d .
O1W O 0.91894(18) 0.14406(19) -0.14502(14) 0.0199(3) Uani 1 1 d .
H1WB H 0.9595 0.2490 -0.1700 0.030 Uiso 1 1 d .
H1WA H 0.9906 0.1032 -0.1678 0.031 Uiso 1 1 d .
O2A O 1.10942(17) 0.13817(17) 0.06971(13) 0.0163(3) Uani 1 1 d .
O2W O 0.6085(2) -0.0381(2) -0.16782(14) 0.0202(4) Uani 1 1 d .
H2WB H 0.527(4) -0.059(4) -0.165(3) 0.044(11) Uiso 1 1 d .
H2WA H 0.641(5) 0.019(5) -0.218(4) 0.067 Uiso 1 1 d .
O2 O 0.85936(18) -0.03742(19) 0.18333(13) 0.0190(3) Uani 1 1 d .
C2A C 1.3872(2) 0.3851(3) 0.17125(18) 0.0150(4) Uani 1 1 d .
H2A H 1.377(3) 0.307(3) 0.202(2) 0.021(7) Uiso 1 1 d .
C2 C 0.7247(3) 0.0721(3) 0.4471(2) 0.0207(5) Uani 1 1 d .
H2 H 0.693(3) 0.146(4) 0.425(2) 0.028(8) Uiso 1 1 d .
N2 N 0.6071(3) 0.2070(3) 0.62043(18) 0.0282(5) Uani 1 1 d .
N2A N 1.6337(2) 0.4200(2) 0.31303(18) 0.0256(5) Uani 1 1 d .
C3A C 1.5265(2) 0.5016(2) 0.18501(18) 0.0150(4) Uani 1 1 d .
C3 C 0.7170(3) 0.0412(3) 0.5538(2) 0.0223(5) Uani 1 1 d .
O3 O 0.9147(2) -0.3401(2) 0.45210(16) 0.0335(4) Uani 1 1 d .
N3 N 0.5531(3) 0.2892(3) 0.6111(2) 0.0399(6) Uani 1 1 d .
N3A N 1.6239(3) 0.3518(3) 0.3783(2) 0.0419(6) Uani 1 1 d .
O3A O 1.32120(18) 0.77003(18) -0.01676(14) 0.0187(3) Uani 1 1 d .
O3W O 1.0354(2) 0.4348(2) -0.17358(18) 0.0342(4) Uani 1 1 d .
H3WB H 1.1366 0.4581 -0.1925 0.051 Uiso 1 1 d .
H3WA H 0.9976 0.5013 -0.1336 0.051 Uiso 1 1 d .
C4 C 0.7635(3) -0.0682(3) 0.5793(2) 0.0229(5) Uani 1 1 d .
H4C H 0.7582 -0.0875 0.6504 0.027 Uiso 1 1 calc R
O4 O 0.8480(3) -0.2938(3) 0.62237(17) 0.0429(6) Uani 1 1 d .
H4B H 0.8682 -0.3661 0.6279 0.064 Uiso 1 1 calc R
C4A C 1.5445(2) 0.6230(2) 0.13844(18) 0.0143(4) Uani 1 1 d .
H4A H 1.638(3) 0.695(3) 0.146(2) 0.023(7) Uiso 1 1 d .
O4A O 1.56862(17) 0.85669(18) 0.03483(14) 0.0192(3) Uani 1 1 d .
O4W O 0.8919(3) -0.5353(3) 0.6347(2) 0.0511(6) Uani 1 1 d .
H4WA H 1.0126 -0.4829 0.6335 0.077 Uiso 1 1 d .
H4WB H 1.0115 -0.4354 0.6502 0.077 Uiso 1 1 d .
C5 C 0.8181(3) -0.1486(3) 0.4981(2) 0.0213(5) Uani 1 1 d .
C5A C 1.4199(2) 0.6320(2) 0.08109(17) 0.0128(4) Uani 1 1 d .
C6A C 1.2784(2) 0.5200(2) 0.07127(18) 0.0139(4) Uani 1 1 d .
H6A H 1.204(3) 0.529(3) 0.036(2) 0.010(6) Uiso 1 1 d .
C6 C 0.8281(3) -0.1176(3) 0.39118(19) 0.0196(5) Uani 1 1 d .
H6 H 0.863(3) -0.177(3) 0.336(2) 0.018(7) Uiso 1 1 d .
C7 C 0.8656(3) -0.2695(3) 0.5212(2) 0.0241(5) Uani 1 1 d .
C7A C 1.4382(2) 0.7621(2) 0.02891(18) 0.0138(4) Uani 1 1 d .
C8A C 1.1139(2) 0.2699(2) 0.09319(17) 0.0136(4) Uani 1 1 d .
C8 C 0.7895(2) 0.0236(3) 0.25007(19) 0.0174(4) Uani 1 1 d .
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'
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_1
_geom_angle_site_symmetry_3
O4A Pr1 O3A 95.47(6) 1_445 2_765
O4A Pr1 O2A 88.15(5) 1_445 2_755
O3A Pr1 O2A 155.27(6) 2_765 2_755
O4A Pr1 O1W 134.47(6) 1_445 .
O3A Pr1 O1W 85.19(5) 2_765 .
O2A Pr1 O1W 75.07(5) 2_755 .
O4A Pr1 O1A 149.57(6) 1_445 .
O3A Pr1 O1A 73.94(5) 2_765 .
O2A Pr1 O1A 113.53(5) 2_755 .
O1W Pr1 O1A 74.09(6) . .
O4A Pr1 O2 76.32(5) 1_445 .
O3A Pr1 O2 126.51(5) 2_765 .
O2A Pr1 O2 78.13(5) 2_755 .
O1W Pr1 O2 137.25(5) . .
O1A Pr1 O2 87.15(6) . .
O4A Pr1 O1 72.26(6) 1_445 .
O3A Pr1 O1 76.06(5) 2_765 .
O2A Pr1 O1 127.98(5) 2_755 .
O1W Pr1 O1 149.33(6) . .
O1A Pr1 O1 77.48(5) . .
O2 Pr1 O1 50.86(5) . .
O4A Pr1 O2W 69.61(6) 1_445 .
O3A Pr1 O2W 73.43(6) 2_765 .
O2A Pr1 O2W 85.08(5) 2_755 .
O1W Pr1 O2W 67.05(6) . .
O1A Pr1 O2W 130.51(6) . .
O2 Pr1 O2W 142.34(6) . .
O1 Pr1 O2W 127.70(5) . .
O4A Pr1 O2A 138.29(5) 1_445 .
O3A Pr1 O2A 121.19(5) 2_765 .
O2A Pr1 O2A 67.17(6) 2_755 .
O1W Pr1 O2A 72.80(5) . .
O1A Pr1 O2A 47.92(5) . .
O2 Pr1 O2A 66.29(5) . .
O1 Pr1 O2A 96.33(5) . .
O2W Pr1 O2A 135.84(5) . .
O4A Pr1 C8 71.64(6) 1_445 .
O3A Pr1 C8 101.35(6) 2_765 .
O2A Pr1 C8 102.99(6) 2_755 .
O1W Pr1 C8 152.88(6) . .
O1A Pr1 C8 82.41(6) . .
O2 Pr1 C8 25.51(6) . .
O1 Pr1 C8 25.38(6) . .
O2W Pr1 C8 140.08(6) . .
O2A Pr1 C8 81.48(5) . .
O4A Pr1 C8A 153.70(6) 1_445 .
O3A Pr1 C8A 96.91(6) 2_765 .
O2A Pr1 C8A 90.20(5) 2_755 .
O1W Pr1 C8A 69.83(6) . .
O1A Pr1 C8A 23.69(5) . .
O2 Pr1 C8A 77.65(6) . .
O1 Pr1 C8A 88.36(6) . .
O2W Pr1 C8A 136.37(6) . .
O2A Pr1 C8A 24.39(5) . .
C8 Pr1 C8A 83.20(6) . .
C8A O1A Pr1 103.13(13) . .
C6A C1A C2A 121.0(2) . .
C6A C1A C8A 118.3(2) . .
C2A C1A C8A 120.6(2) . .
C8 O1 Pr1 91.91(13) . .
C6 C1 C2 120.1(2) . .
C6 C1 C8 120.2(2) . .
C2 C1 C8 119.7(2) . .
N2A N1A C3A 115.4(2) . .
N2 N1 C3 116.7(2) . .
Pr1 O1W H1WB 135.5 . .
Pr1 O1W H1WA 112.6 . .
H1WB O1W H1WA 103.1 . .
C8A O2A Pr1 152.23(14) . 2_755
C8A O2A Pr1 86.72(12) . .
Pr1 O2A Pr1 112.83(6) 2_755 .
Pr1 O2W H2WB 120(3) . .
Pr1 O2W H2WA 113(3) . .
H2WB O2W H2WA 111(4) . .
C8 O2 Pr1 95.57(14) . .
C3A C2A C1A 119.2(2) . .
C3A C2A H2A 119.6(18) . .
C1A C2A H2A 121.1(18) . .
C3 C2 C1 119.2(2) . .
C3 C2 H2 123.9(18) . .
C1 C2 H2 116.9(18) . .
N3 N2 N1 172.4(3) . .
N3A N2A N1A 173.9(3) . .
C4A C3A C2A 120.3(2) . .
C4A C3A N1A 116.54(19) . .
C2A C3A N1A 123.2(2) . .
C4 C3 C2 120.9(2) . .
C4 C3 N1 115.2(2) . .
C2 C3 N1 124.0(2) . .
C7A O3A Pr1 138.01(14) . 2_765
H3WB O3W H3WA 125.6 . .
C3 C4 C5 119.8(2) . .
C3 C4 H4C 120.1 . .
C5 C4 H4C 120.1 . .
C7 O4 H4B 109.5 . .
C3A C4A C5A 119.8(2) . .
C3A C4A H4A 118.1(18) . .
C5A C4A H4A 122.1(18) . .
C7A O4A Pr1 167.99(15) . 1_665
H4WA O4W H4WB 23.7 . .
C4 C5 C6 120.0(2) . .
C4 C5 C7 121.5(2) . .
C6 C5 C7 118.5(2) . .
C6A C5A C4A 120.6(2) . .
C6A C5A C7A 119.04(19) . .
C4A C5A C7A 120.37(19) . .
C1A C6A C5A 118.9(2) . .
C1A C6A H6A 122.6(17) . .
C5A C6A H6A 118.4(17) . .
C1 C6 C5 120.2(2) . .
C1 C6 H6 121.6(16) . .
C5 C6 H6 118.2(16) . .
O3 C7 O4 123.0(2) . .
O3 C7 C5 122.7(2) . .
O4 C7 C5 114.3(2) . .
O4A C7A O3A 124.6(2) . .
O4A C7A C5A 117.03(19) . .
O3A C7A C5A 118.33(18) . .
O1A C8A O2A 121.45(19) . .
O1A C8A C1A 119.08(19) . .
O2A C8A C1A 119.45(19) . .
O1A C8A Pr1 53.19(11) . .
O2A C8A Pr1 68.90(11) . .
C1A C8A Pr1 167.56(15) . .
O1 C8 O2 121.5(2) . .
O1 C8 C1 121.0(2) . .
O2 C8 C1 117.5(2) . .
O1 C8 Pr1 62.70(12) . .
O2 C8 Pr1 58.92(11) . .
C1 C8 Pr1 173.76(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pr1 O4A 2.3571(15) 1_445
Pr1 O3A 2.3905(16) 2_765
Pr1 O2A 2.4662(16) 2_755
Pr1 O1W 2.5044(16) .
Pr1 O1A 2.5204(16) .
Pr1 O2 2.5327(16) .
Pr1 O1 2.6170(16) .
Pr1 O2W 2.6415(18) .
Pr1 O2A 2.8650(16) .
Pr1 C8 2.943(2) .
Pr1 C8A 3.066(2) .
O1A C8A 1.265(3) .
C1A C6A 1.387(3) .
C1A C2A 1.410(3) .
C1A C8A 1.502(3) .
O1 C8 1.262(3) .
C1 C6 1.392(3) .
C1 C2 1.404(3) .
C1 C8 1.514(3) .
N1A N2A 1.242(3) .
N1A C3A 1.449(3) .
N1 N2 1.256(3) .
N1 C3 1.436(3) .
O1W H1WB 1.0771 .
O1W H1WA 0.9375 .
O2A C8A 1.268(3) .
O2A Pr1 2.4662(16) 2_755
O2W H2WB 0.73(4) .
O2W H2WA 0.90(5) .
O2 C8 1.274(3) .
C2A C3A 1.397(3) .
C2A H2A 0.90(3) .
C2 C3 1.402(3) .
C2 H2 0.96(3) .
N2 N3 1.129(3) .
N2A N3A 1.127(3) .
C3A C4A 1.384(3) .
C3 C4 1.391(4) .
O3 C7 1.213(3) .
O3A C7A 1.275(3) .
O3A Pr1 2.3905(16) 2_765
O3W H3WB 0.9573 .
O3W H3WA 0.9321 .
C4 C5 1.393(3) .
C4 H4C 0.9300 .
O4 C7 1.316(3) .
O4 H4B 0.8200 .
C4A C5A 1.410(3) .
C4A H4A 0.91(3) .
O4A C7A 1.254(3) .
O4A Pr1 2.3571(15) 1_665
O4W H4WA 1.0853 .
O4W H4WB 1.1974 .
C5 C6 1.405(3) .
C5 C7 1.494(3) .
C5A C6A 1.394(3) .
C5A C7A 1.501(3) .
C6A H6A 0.87(3) .
C6 H6 0.96(3) .
