#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:43:35 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180352 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/21/7202125.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_7202125
loop_
_publ_author_name
'Kong, Xiang-Jian'
'Ren, Yan-Ping'
'Long, La-Sheng'
'Huang, Rong-Bin'
'Zheng, Lan-Sun'
'Kurmoo, Mohamedally'
_publ_section_title
;
 Influence of reaction conditions on the channel shape of 3d-4f
 heterometallic metal--organic framework
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1309
_journal_paper_doi               10.1039/b804966a
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C18 H28 N4 Ni2 O24 Pr2'
_chemical_formula_weight         1083.68
_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                74.748(5)
_cell_angle_beta                 88.024(5)
_cell_angle_gamma                86.919(5)
_cell_formula_units_Z            1
_cell_length_a                   7.113(2)
_cell_length_b                   8.519(2)
_cell_length_c                   12.641(4)
_cell_measurement_reflns_used    3460
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.403
_cell_measurement_theta_min      2.481
_cell_volume                     737.8(4)
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3094
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    4.612
_exptl_absorpt_correction_T_max  0.7384
_exptl_absorpt_correction_T_min  0.4168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       stick
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.127
_refine_diff_density_min         -2.314
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0916P)²+1.4296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                2310
_reflns_number_total             2363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b804966a.txt
_cod_data_source_block           complex5
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7202125
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.20527(2) 0.06631(2) 0.685363(14) 0.00791(6) Uani 1 1 d . . .
Ni1 Ni -0.5000 0.0000 1.0000 0.00864(15) Uani 1 2 d S . .
Ni2 Ni -0.5000 0.5000 0.5000 0.00893(15) Uani 1 2 d S . .
O1 O -0.0521(4) 0.0665(4) 0.8023(2) 0.0216(7) Uani 1 1 d . . .
O2 O -0.2889(4) 0.1132(3) 0.9053(2) 0.0160(7) Uani 1 1 d . . .
C1 C -0.1953(6) -0.1596(5) 0.9136(4) 0.0242(11) Uani 1 1 d . . .
H1A H -0.2023 -0.2082 0.8509 0.029 Uiso 1 1 calc R . .
H1B H -0.0799 -0.2060 0.9541 0.029 Uiso 1 1 calc R . .
C2 C -0.1796(5) 0.0209(5) 0.8704(3) 0.0144(9) Uani 1 1 d . . .
N1 N -0.3577(4) -0.2052(4) 0.9855(3) 0.0112(7) Uani 1 1 d . . .
H1C H -0.3189 -0.2670 1.0540 0.013 Uiso 1 1 calc R . .
C3 C -0.4959(6) -0.2911(5) 0.9430(3) 0.0175(10) Uani 1 1 d . . .
H3A H -0.5694 -0.3581 1.0049 0.021 Uiso 1 1 calc R . .
H3B H -0.4300 -0.3653 0.9039 0.021 Uiso 1 1 calc R . .
C4 C -0.6264(6) -0.1764(5) 0.8668(3) 0.0145(9) Uani 1 1 d . . .
O3 O -0.7337(4) -0.2267(3) 0.8100(2) 0.0148(6) Uani 1 1 d . . .
O4 O -0.6214(4) -0.0277(3) 0.8623(2) 0.0137(6) Uani 1 1 d . . .
O5 O -0.0107(4) 0.2538(3) 0.5742(2) 0.0165(7) Uani 1 1 d . . .
O6 O -0.2661(4) 0.3580(3) 0.4869(2) 0.0112(6) Uani 1 1 d . . .
C5 C -0.1908(5) 0.4375(5) 0.6466(3) 0.0152(9) Uani 1 1 d . . .
H5A H -0.1938 0.3608 0.7206 0.018 Uiso 1 1 calc R . .
H5B H -0.0849 0.5095 0.6435 0.018 Uiso 1 1 calc R . .
C6 C -0.1554(5) 0.3426(5) 0.5633(3) 0.0124(9) Uani 1 1 d . . .
N2 N -0.3674(4) 0.5372(4) 0.6308(3) 0.0113(7) Uani 1 1 d . . .
H2A H -0.3416 0.6466 0.6176 0.014 Uiso 1 1 calc R . .
C7 C -0.5026(5) 0.4934(5) 0.7216(3) 0.0106(8) Uani 1 1 d . . .
H7A H -0.5822 0.5909 0.7251 0.013 Uiso 1 1 calc R . .
H7B H -0.4343 0.4552 0.7913 0.013 Uiso 1 1 calc R . .
C8 C -0.6244(5) 0.3633(5) 0.7088(3) 0.0133(9) Uani 1 1 d . . .
O7 O -0.6020(4) 0.3136(3) 0.6225(2) 0.0122(6) Uani 1 1 d . . .
O8 O -0.7397(4) 0.3012(3) 0.7810(2) 0.0143(6) Uani 1 1 d . . .
C9 C 0.5644(5) -0.0465(4) 0.5459(3) 0.0112(8) Uani 1 1 d . . .
O9 O 0.5093(4) -0.0599(4) 0.6404(2) 0.0165(7) Uani 1 1 d . . .
O10 O 0.7145(3) -0.1054(3) 0.5163(2) 0.0122(6) Uani 1 1 d . . .
O1W O 0.0427(4) -0.1412(3) 0.6244(2) 0.0159(7) Uani 1 1 d . . .
H1WA H 0.0715 -0.2226 0.6756 0.019 Uiso 1 1 d R . .
H1WB H -0.0739 -0.1497 0.6254 0.019 Uiso 1 1 d R . .
O2W O 0.0184(13) -0.4941(10) 0.8805(8) 0.060(3) Uani 0.50 1 d P . .
O2W' O 0.0964(16) -0.4498(14) 1.0947(7) 0.067(3) Uani 0.50 1 d P . .
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'
Ni Ni 0.3393 1.1124 '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
_geom_angle_publ_flag
O1 Pr1 O5 77.22(10) . . ?
O1 Pr1 O1W 85.46(11) . . ?
O5 Pr1 O1W 84.99(10) . . ?
O1 Pr1 O9 150.06(9) . . ?
O5 Pr1 O9 131.47(9) . . ?
O1W Pr1 O9 88.62(10) . . ?
O1 Pr1 O7 120.50(10) . 1_655 ?
O5 Pr1 O7 78.50(9) . 1_655 ?
O1W Pr1 O7 144.38(9) . 1_655 ?
O9 Pr1 O7 79.44(9) . 1_655 ?
O1 Pr1 O4 82.70(10) . 1_655 ?
O5 Pr1 O4 148.96(10) . 1_655 ?
O1W Pr1 O4 116.95(9) . 1_655 ?
O9 Pr1 O4 73.95(9) . 1_655 ?
O7 Pr1 O4 91.95(9) 1_655 1_655 ?
O1 Pr1 O10 140.62(9) . 2_656 ?
O5 Pr1 O10 68.71(9) . 2_656 ?
O1W Pr1 O10 72.76(9) . 2_656 ?
O9 Pr1 O10 63.48(8) . 2_656 ?
O7 Pr1 O10 71.87(9) 1_655 2_656 ?
O4 Pr1 O10 136.34(8) 1_655 2_656 ?
O1 Pr1 O3 83.05(9) . 1_655 ?
O5 Pr1 O3 146.80(9) . 1_655 ?
O1W Pr1 O3 66.90(9) . 1_655 ?
O9 Pr1 O3 67.69(9) . 1_655 ?
O7 Pr1 O3 134.70(9) 1_655 1_655 ?
O4 Pr1 O3 50.27(9) 1_655 1_655 ?
O10 Pr1 O3 115.78(9) 2_656 1_655 ?
O1 Pr1 O8 74.86(10) . 1_655 ?
O5 Pr1 O8 85.89(10) . 1_655 ?
O1W Pr1 O8 159.72(9) . 1_655 ?
O9 Pr1 O8 110.89(9) . 1_655 ?
O7 Pr1 O8 49.88(8) 1_655 1_655 ?
O4 Pr1 O8 65.99(9) 1_655 1_655 ?
O10 Pr1 O8 120.20(8) 2_656 1_655 ?
O3 Pr1 O8 114.46(9) 1_655 1_655 ?
O1 Pr1 C4 85.62(10) . 1_655 ?
O5 Pr1 C4 162.75(10) . 1_655 ?
O1W Pr1 C4 92.03(11) . 1_655 ?
O9 Pr1 C4 65.27(10) . 1_655 ?
O7 Pr1 C4 112.41(10) 1_655 1_655 ?
O4 Pr1 C4 25.57(11) 1_655 1_655 ?
O10 Pr1 C4 126.54(10) 2_656 1_655 ?
O3 Pr1 C4 25.15(11) 1_655 1_655 ?
O8 Pr1 C4 91.33(10) 1_655 1_655 ?
O1 Pr1 C8 98.40(11) . 1_655 ?
O5 Pr1 C8 83.62(11) . 1_655 ?
O1W Pr1 C8 166.84(10) . 1_655 ?
O9 Pr1 C8 93.99(10) . 1_655 ?
O7 Pr1 C8 25.32(10) 1_655 1_655 ?
O4 Pr1 C8 76.12(10) 1_655 1_655 ?
O10 Pr1 C8 96.88(10) 2_656 1_655 ?
O3 Pr1 C8 125.93(10) 1_655 1_655 ?
O8 Pr1 C8 24.74(9) 1_655 1_655 ?
C4 Pr1 C8 100.78(11) 1_655 1_655 ?
O2 Ni1 O2 180.0 2_457 . ?
O2 Ni1 N1 95.93(12) 2_457 . ?
O2 Ni1 N1 84.07(12) . . ?
O2 Ni1 N1 84.07(12) 2_457 2_457 ?
O2 Ni1 N1 95.93(12) . 2_457 ?
N1 Ni1 N1 180.00(18) . 2_457 ?
O2 Ni1 O4 91.04(11) 2_457 . ?
O2 Ni1 O4 88.96(11) . . ?
N1 Ni1 O4 80.47(12) . . ?
N1 Ni1 O4 99.53(12) 2_457 . ?
O2 Ni1 O4 88.96(11) 2_457 2_457 ?
O2 Ni1 O4 91.04(11) . 2_457 ?
N1 Ni1 O4 99.53(12) . 2_457 ?
N1 Ni1 O4 80.47(12) 2_457 2_457 ?
O4 Ni1 O4 180.000(1) . 2_457 ?
O6 Ni2 O6 180.0 . 2_466 ?
O6 Ni2 N2 95.95(12) . 2_466 ?
O6 Ni2 N2 84.05(12) 2_466 2_466 ?
O6 Ni2 N2 84.05(12) . . ?
O6 Ni2 N2 95.95(12) 2_466 . ?
N2 Ni2 N2 180.000(1) 2_466 . ?
O6 Ni2 O7 89.58(10) . . ?
O6 Ni2 O7 90.42(10) 2_466 . ?
N2 Ni2 O7 100.06(12) 2_466 . ?
N2 Ni2 O7 79.94(12) . . ?
O6 Ni2 O7 90.42(10) . 2_466 ?
O6 Ni2 O7 89.58(10) 2_466 2_466 ?
N2 Ni2 O7 79.94(12) 2_466 2_466 ?
N2 Ni2 O7 100.06(12) . 2_466 ?
O7 Ni2 O7 180.000(1) . 2_466 ?
C2 O1 Pr1 162.3(3) . . ?
C2 O2 Ni1 113.7(3) . . ?
N1 C1 C2 113.6(3) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
O2 C2 O1 124.2(4) . . ?
O2 C2 C1 119.4(3) . . ?
O1 C2 C1 116.4(4) . . ?
C1 N1 C3 114.3(3) . . ?
C1 N1 Ni1 108.5(2) . . ?
C3 N1 Ni1 103.9(2) . . ?
C1 N1 H1C 110.0 . . ?
C3 N1 H1C 110.0 . . ?
Ni1 N1 H1C 110.0 . . ?
N1 C3 C4 111.6(3) . . ?
N1 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 O4 121.8(4) . . ?
O3 C4 C3 120.7(4) . . ?
O4 C4 C3 117.5(4) . . ?
O3 C4 Pr1 63.8(2) . 1_455 ?
O4 C4 Pr1 59.8(2) . 1_455 ?
C3 C4 Pr1 165.5(3) . 1_455 ?
C4 O3 Pr1 91.1(2) . 1_455 ?
C4 O4 Ni1 109.8(2) . . ?
C4 O4 Pr1 94.7(2) . 1_455 ?
Ni1 O4 Pr1 155.29(13) . 1_455 ?
C6 O5 Pr1 151.0(3) . . ?
C6 O6 Ni2 113.2(2) . . ?
N2 C5 C6 113.5(3) . . ?
N2 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
O5 C6 O6 123.4(4) . . ?
O5 C6 C5 116.3(4) . . ?
O6 C6 C5 120.3(3) . . ?
C7 N2 C5 114.2(3) . . ?
C7 N2 Ni2 104.7(2) . . ?
C5 N2 Ni2 108.5(2) . . ?
C7 N2 H2A 109.7 . . ?
C5 N2 H2A 109.7 . . ?
Ni2 N2 H2A 109.7 . . ?
N2 C7 C8 111.4(3) . . ?
N2 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O8 C8 O7 120.7(4) . . ?
O8 C8 C7 121.4(4) . . ?
O7 C8 C7 117.9(3) . . ?
O8 C8 Pr1 63.7(2) . 1_455 ?
O7 C8 Pr1 57.61(19) . 1_455 ?
C7 C8 Pr1 168.5(3) . 1_455 ?
C8 O7 Ni2 108.1(2) . . ?
C8 O7 Pr1 97.1(2) . 1_455 ?
Ni2 O7 Pr1 150.68(14) . 1_455 ?
C8 O8 Pr1 91.5(2) . 1_455 ?
O9 C9 O10 126.4(4) . . ?
O9 C9 C9 117.7(4) . 2_656 ?
O10 C9 C9 115.8(4) . 2_656 ?
C9 O9 Pr1 122.3(2) . . ?
C9 O10 Pr1 120.6(2) . 2_656 ?
Pr1 O1W H1WA 99.0 . . ?
Pr1 O1W H1WB 125.4 . . ?
H1WA O1W H1WB 99.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O1 2.313(3) . ?
Pr1 O5 2.364(3) . ?
Pr1 O1W 2.460(3) . ?
Pr1 O9 2.479(3) . ?
Pr1 O7 2.511(3) 1_655 ?
Pr1 O4 2.512(3) 1_655 ?
Pr1 O10 2.531(3) 2_656 ?
Pr1 O3 2.600(3) 1_655 ?
Pr1 O8 2.647(3) 1_655 ?
Pr1 C4 2.898(4) 1_655 ?
Pr1 C8 2.951(4) 1_655 ?
Ni1 O2 2.011(3) 2_457 ?
Ni1 O2 2.011(3) . ?
Ni1 N1 2.020(3) . ?
Ni1 N1 2.020(3) 2_457 ?
Ni1 O4 2.042(3) . ?
Ni1 O4 2.042(3) 2_457 ?
Ni2 O6 2.032(3) . ?
Ni2 O6 2.032(3) 2_466 ?
Ni2 N2 2.035(3) 2_466 ?
Ni2 N2 2.035(3) . ?
Ni2 O7 2.049(3) . ?
Ni2 O7 2.049(3) 2_466 ?
O1 C2 1.234(5) . ?
O2 C2 1.228(5) . ?
C1 N1 1.449(5) . ?
C1 C2 1.499(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N1 C3 1.453(5) . ?
N1 H1C 0.9300 . ?
C3 C4 1.488(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.232(5) . ?
C4 O4 1.255(5) . ?
C4 Pr1 2.898(4) 1_455 ?
O3 Pr1 2.600(3) 1_455 ?
O4 Pr1 2.512(3) 1_455 ?
O5 C6 1.234(5) . ?
O6 C6 1.243(5) . ?
C5 N2 1.467(5) . ?
C5 C6 1.494(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
N2 C7 1.455(5) . ?
N2 H2A 0.9300 . ?
C7 C8 1.488(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O8 1.235(5) . ?
C8 O7 1.272(5) . ?
C8 Pr1 2.951(4) 1_455 ?
O7 Pr1 2.511(3) 1_455 ?
O8 Pr1 2.647(3) 1_455 ?
C9 O9 1.222(5) . ?
C9 O10 1.243(5) . ?
C9 C9 1.526(8) 2_656 ?
O10 Pr1 2.531(3) 2_656 ?
O1W H1WA 0.8360 . ?
O1W H1WB 0.8363 . ?
O2W O2W' 0.969(13) 2_547 ?
O2W' O2W 0.969(13) 2_547 ?
