#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:05:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180411 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/80/7208036.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_7208036
loop_
_publ_author_name
'Pan, Yingyi'
'Ma, Deyun'
'Liu, Huimin'
'Wu, Hao'
'He, Dehua'
'Li, Yingwei'
_publ_section_title
;
 Uncoordinated carbonyl groups of MOFs as anchoring sites for the
 preparation of highly active Pd nano-catalysts
;
_journal_issue                   21
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              10834
_journal_paper_doi               10.1039/c2jm30867c
_journal_volume                  22
_journal_year                    2012
_chemical_formula_moiety         'C9 H13 N3 O11 Tm'
_chemical_formula_sum            'C9 H13 N3 O11 Tm'
_chemical_formula_weight         508.15
_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                118.8290(10)
_cell_angle_beta                 90.6090(10)
_cell_angle_gamma                91.6870(10)
_cell_formula_units_Z            2
_cell_length_a                   6.0200(5)
_cell_length_b                   12.7722(11)
_cell_length_c                   13.1612(11)
_cell_measurement_reflns_used    3500
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.26
_cell_volume                     885.79(13)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-XP (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4623
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.064
_exptl_absorpt_correction_T_max  0.357
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3147
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0402
_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)+(0.0519P)²+3.9259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                2771
_reflns_number_total             3147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2jm30867c.txt
_cod_data_source_block           Tm
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7208036
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
C1 C 0.6106(14) 0.5189(7) 0.0945(7) 0.0221(18) Uani 1 1 d .
H1 H 0.6928 0.5341 0.1607 0.027 Uiso 1 1 calc R
N1 N 0.4236(11) 0.4522(6) 0.0699(6) 0.0215(15) Uani 1 1 d .
O1 O 0.0497(9) 0.3209(5) 0.0147(5) 0.0250(13) Uani 1 1 d .
Tm1 Tm 0.22197(5) 0.33935(3) 0.17829(3) 0.01648(13) Uani 1 1 d .
C2 C 0.3116(14) 0.4337(7) -0.0276(7) 0.0222(18) Uani 1 1 d .
N2 N 0.0703(11) 0.1211(6) 0.0558(6) 0.0199(14) Uani 1 1 d .
O2 O -0.0202(11) 0.3444(6) -0.1388(5) 0.0333(15) Uani 1 1 d .
C3 C 0.0960(13) 0.3600(7) -0.0544(7) 0.0206(17) Uani 1 1 d .
N3 N 0.0858(11) 0.4269(6) 0.3914(5) 0.0196(14) Uani 1 1 d .
O3 O 0.3066(10) 0.2144(5) 0.2520(5) 0.0281(14) Uani 1 1 d .
C4 C 0.1173(14) 0.0493(7) 0.1000(7) 0.0236(18) Uani 1 1 d .
C5 C -0.0473(14) 0.0712(7) -0.0447(7) 0.0254(19) Uani 1 1 d .
H5 H -0.0832 0.1181 -0.0785 0.030 Uiso 1 1 calc R
C6 C 0.2498(16) 0.1070(8) 0.2131(7) 0.030(2) Uani 1 1 d .
O1W O 0.4945(9) 0.2213(5) 0.0510(5) 0.0277(13) Uani 1 1 d D
H1W H 0.6206 0.2482 0.0823 0.041 Uiso 1 1 d RD
H2W H 0.4950 0.2095 -0.0175 0.041 Uiso 1 1 d RD
O2W O 0.1295(10) 0.5409(5) 0.2590(5) 0.0303(14) Uani 1 1 d D
H3W H 0.1963 0.5956 0.3179 0.045 Uiso 1 1 d RD
H4W H 0.0705 0.5705 0.2211 0.045 Uiso 1 1 d RD
O3W O 0.273(8) 0.149(4) 0.591(6) 0.96(9) Uani 1 1 d D
H5W H 0.1390 0.1428 0.5986 1.442 Uiso 1 1 d RD
H6W H 0.3092 0.2099 0.5875 1.442 Uiso 1 1 d RD
O4W O 0.786(5) 0.2898(12) 0.5291(12) 0.270(15) Uani 1 1 d D
H7W H 0.9030 0.2623 0.5354 0.405 Uiso 1 1 d RD
H8W H 0.6778 0.2672 0.5514 0.405 Uiso 1 1 d RD
O5W O 0.4197(13) 0.8029(7) 0.1672(6) 0.054(2) Uani 1 1 d D
H9W H 0.3067 0.8302 0.1517 0.081 Uiso 1 1 d RD
H10W H 0.5318 0.8464 0.1729 0.081 Uiso 1 1 d RD
O4 O 0.3004(16) 0.0440(6) 0.2562(7) 0.063(3) Uani 1 1 d .
O6 O -0.4631(9) 0.4311(5) 0.2960(5) 0.0232(13) Uani 1 1 d .
O5 O -0.1643(9) 0.3342(5) 0.2031(5) 0.0253(13) Uani 1 1 d .
C7 C -0.1239(12) 0.4604(7) 0.4034(7) 0.0174(16) Uani 1 1 d .
C8 C 0.2084(13) 0.4652(7) 0.4894(7) 0.0192(17) Uani 1 1 d .
H8 H 0.3538 0.4410 0.4849 0.023 Uiso 1 1 calc R
C9 C -0.2618(13) 0.4059(7) 0.2939(7) 0.0181(16) Uiso 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'
Tm Tm -0.3139 5.2483 '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 C1 C2 123.5(7) . 2_665
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 2_665 .
C1 N1 C2 115.3(7) . .
C1 N1 Tm1 131.8(5) . .
C2 N1 Tm1 112.9(5) . .
C3 O1 Tm1 133.4(5) . .
O1 Tm1 O3 136.6(2) . .
O1 Tm1 O6 140.04(19) . 1_655
O3 Tm1 O6 76.1(2) . 1_655
O1 Tm1 O2W 84.1(2) . .
O3 Tm1 O2W 134.9(2) . .
O6 Tm1 O2W 80.0(2) 1_655 .
O1 Tm1 O1W 84.8(2) . .
O3 Tm1 O1W 78.0(2) . .
O6 Tm1 O1W 81.02(19) 1_655 .
O2W Tm1 O1W 134.8(2) . .
O1 Tm1 O5 72.4(2) . .
O3 Tm1 O5 96.0(2) . .
O6 Tm1 O5 136.83(19) 1_655 .
O2W Tm1 O5 76.4(2) . .
O1W Tm1 O5 139.7(2) . .
O1 Tm1 N2 71.5(2) . .
O3 Tm1 N2 65.1(2) . .
O6 Tm1 N2 135.1(2) 1_655 .
O2W Tm1 N2 144.1(2) . .
O1W Tm1 N2 69.9(2) . .
O5 Tm1 N2 71.5(2) . .
O1 Tm1 N3 131.1(2) . .
O3 Tm1 N3 69.7(2) . .
O6 Tm1 N3 74.8(2) 1_655 .
O2W Tm1 N3 67.4(2) . .
O1W Tm1 N3 143.2(2) . .
O5 Tm1 N3 62.94(19) . .
N2 Tm1 N3 109.6(2) . .
O1 Tm1 N1 62.69(19) . .
O3 Tm1 N1 139.8(2) . .
O6 Tm1 N1 77.36(19) 1_655 .
O2W Tm1 N1 67.5(2) . .
O1W Tm1 N1 68.5(2) . .
O5 Tm1 N1 123.8(2) . .
N2 Tm1 N1 119.4(2) . .
N3 Tm1 N1 130.0(2) . .
N1 C2 C1 121.2(8) . 2_665
N1 C2 C3 115.4(7) . .
C1 C2 C3 123.4(7) 2_665 .
C4 N2 C5 116.4(7) . .
C4 N2 Tm1 114.6(5) . .
C5 N2 Tm1 129.0(5) . .
O2 C3 O1 125.5(7) . .
O2 C3 C2 118.9(7) . .
O1 C3 C2 115.6(7) . .
C7 N3 C8 116.5(7) . .
C7 N3 Tm1 113.4(5) . .
C8 N3 Tm1 128.3(5) . .
C6 O3 Tm1 128.4(5) . .
N2 C4 C5 121.9(8) . 2
N2 C4 C6 115.6(7) . .
C5 C4 C6 122.5(7) 2 .
N2 C5 C4 121.7(7) . 2
N2 C5 H5 119.1 . .
C4 C5 H5 119.1 2 .
O4 C6 O3 125.7(8) . .
O4 C6 C4 118.0(8) . .
O3 C6 C4 116.2(7) . .
Tm1 O1W H1W 108.8 . .
Tm1 O1W H2W 120.1 . .
H1W O1W H2W 109.1 . .
Tm1 O2W H3W 122.4 . .
Tm1 O2W H4W 123.9 . .
H3W O2W H4W 109.1 . .
H5W O3W H6W 113.2 . .
H7W O4W H8W 114.3 . .
H9W O5W H10W 109.2 . .
C9 O6 Tm1 135.4(5) . 1_455
C9 O5 Tm1 124.3(5) . .
N3 C7 C8 121.9(7) . 2_566
N3 C7 C9 115.0(7) . .
C8 C7 C9 123.1(7) 2_566 .
N3 C8 C7 121.6(7) . 2_566
N3 C8 H8 119.2 . .
C7 C8 H8 119.2 2_566 .
O6 C9 O5 124.1(7) . .
O6 C9 C7 120.0(7) . .
O5 C9 C7 115.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.329(10) .
C1 C2 1.366(11) 2_665
C1 H1 0.9300 .
N1 C2 1.356(10) .
N1 Tm1 2.740(6) .
O1 C3 1.262(9) .
O1 Tm1 2.283(5) .
Tm1 O3 2.298(6) .
Tm1 O6 2.329(5) 1_655
Tm1 O2W 2.350(6) .
Tm1 O1W 2.354(6) .
Tm1 O5 2.355(6) .
Tm1 N2 2.586(6) .
Tm1 N3 2.620(6) .
C2 C1 1.366(11) 2_665
C2 C3 1.515(11) .
N2 C4 1.337(10) .
N2 C5 1.341(10) .
O2 C3 1.234(10) .
N3 C7 1.332(10) .
N3 C8 1.341(10) .
O3 C6 1.245(10) .
C4 C5 1.397(11) 2
C4 C6 1.509(11) .
C5 C4 1.397(11) 2
C5 H5 0.9300 .
C6 O4 1.230(11) .
O1W H1W 0.8400 .
O1W H2W 0.8400 .
O2W H3W 0.8400 .
O2W H4W 0.8400 .
O3W H5W 0.8203 .
O3W H6W 0.8212 .
O4W H7W 0.8164 .
O4W H8W 0.8175 .
O5W H9W 0.8400 .
O5W H10W 0.8401 .
O6 C9 1.260(9) .
O6 Tm1 2.329(5) 1_455
O5 C9 1.266(9) .
C7 C8 1.380(11) 2_566
C7 C9 1.491(11) .
C8 C7 1.380(11) 2_566
C8 H8 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2W H4W O2 0.84 1.90 2.712(8) 163.7 2_565
O2W H3W O4W 0.84 1.83 2.608(15) 153.1 2_666
O1W H2W O5W 0.84 1.97 2.792(9) 164.6 2_665
O1W H1W O5 0.84 1.90 2.694(8) 158.0 1_655
