#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:12:28 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179050 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/12/4301264.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_4301264
loop_
_publ_author_name
'Lijun Han'
'Suojiang Zhang'
'Yibo Wang'
'Xingjuan Yan'
'Xingmei Lu'
_publ_section_title
;
A Strategy for Synthesis of Ionic Metal-Organic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              786
_journal_page_last               788
_journal_paper_doi               10.1021/ic800632r
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C7 H17 Br Cl N2 O7 Pr'
_chemical_formula_sum            'C7 H17 Br Cl N2 O7 Pr'
_chemical_formula_weight         497.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 96.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7533(18)
_cell_length_b                   17.854(4)
_cell_length_c                   8.6180(17)
_cell_measurement_reflns_used    774
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.3
_cell_volume                     1339.2(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.496
_diffrn_measured_fraction_theta_max 0.496
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3097
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.850
_exptl_absorpt_correction_T_max  0.4070
_exptl_absorpt_correction_T_min  0.2178
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'numabs (Riaku, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0056(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         817
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0243
_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)+(0.0423P)²+2.5539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                782
_reflns_number_total             817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800632r_si_001_2.cif
_cod_data_source_block           shelxl1
_cod_original_cell_volume        1339.3(5)
_cod_database_code               4301264
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.67152(3) 0.0000 0.22535(4) 0.00853(19) Uani 1 2 d S . .
Cl1 Cl 0.98910(17) 0.0000 0.26826(19) 0.0132(3) Uani 1 2 d S A .
C1 C 0.6681(5) 0.0998(3) -0.1372(5) 0.0107(9) Uani 1 1 d . . .
C2 C 0.7794(5) 0.1527(3) -0.2064(5) 0.0120(9) Uani 1 1 d . A .
H2A H 0.8256 0.1267 -0.2915 0.014 Uiso 1 1 calc R . .
H2B H 0.7219 0.1966 -0.2522 0.014 Uiso 1 1 calc R . .
C3 C 1.0000 0.1355(4) 0.0000 0.0115(12) Uani 1 2 d S . .
H3 H 1.0000 0.0823 0.0000 0.014 Uiso 1 2 calc SR . .
C4 C 0.9280(7) 0.2524(4) -0.0683(8) 0.0273(14) Uani 1 1 d U . .
H4 H 0.8756 0.2936 -0.1194 0.033 Uiso 1 1 calc R . .
N1 N 0.9032(4) 0.1790(2) -0.0896(5) 0.0118(8) Uani 1 1 d . . .
O1 O 0.6895(4) 0.0808(2) 0.0018(4) 0.0148(7) Uani 1 1 d . A .
O2 O 0.4421(4) 0.0789(2) 0.2352(4) 0.0181(7) Uani 1 1 d . . .
H2C H 0.4521 0.1248 0.2601 0.027 Uiso 1 1 d R . .
H2D H 0.3531 0.0602 0.2136 0.027 Uiso 1 1 d R . .
O4 O 0.7317(4) -0.1324(2) 0.3363(5) 0.0234(8) Uani 1 1 d . A .
H4A H 0.6696 -0.1559 0.3863 0.035 Uiso 1 1 d R . .
H4B H 0.8109 -0.1520 0.3782 0.035 Uiso 1 1 d R . .
Br1 Br 0.0000 0.24548(4) 0.5000 0.0205(2) Uani 1 2 d S . .
O3 O 0.7051(12) 0.0000 0.5106(12) 0.0178(16) Uani 0.540(12) 2 d SP A 1
H3A H 0.7949 0.0000 0.5590 0.027 Uiso 0.540(12) 2 d SPR A 1
H3B H 0.6270 0.0000 0.5614 0.027 Uiso 0.540(12) 2 d SPR A 1
O3' O 0.6296(15) 0.0000 0.5032(14) 0.0178(16) Uani 0.460(12) 2 d SP A 2
H3'A H 0.7058 0.0000 0.5730 0.027 Uiso 0.460(12) 2 d SPR A 2
H3'B H 0.5386 0.0000 0.5292 0.027 Uiso 0.460(12) 2 d SPR A 2
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pr1 O1 72.97(17) 6 . ?
O1 Pr1 O3 141.99(10) 6 . ?
O1 Pr1 O3 141.99(10) . . ?
O1 Pr1 O2 79.00(12) 6 6 ?
O1 Pr1 O2 119.32(11) . 6 ?
O3 Pr1 O2 88.7(2) . 6 ?
O1 Pr1 O2 119.32(11) 6 . ?
O1 Pr1 O2 79.00(12) . . ?
O3 Pr1 O2 88.7(2) . . ?
O2 Pr1 O2 69.81(18) 6 . ?
O1 Pr1 O3' 143.33(9) 6 . ?
O1 Pr1 O3' 143.33(9) . . ?
O3 Pr1 O3' 15.4(3) . . ?
O2 Pr1 O3' 76.1(3) 6 . ?
O2 Pr1 O3' 76.1(3) . . ?
O1 Pr1 O4 144.13(13) 6 6 ?
O1 Pr1 O4 73.87(12) . 6 ?
O3 Pr1 O4 68.26(10) . 6 ?
O2 Pr1 O4 130.23(12) 6 6 ?
O2 Pr1 O4 66.34(12) . 6 ?
O3' Pr1 O4 71.66(12) . 6 ?
O1 Pr1 O4 73.87(12) 6 . ?
O1 Pr1 O4 144.13(13) . . ?
O3 Pr1 O4 68.26(10) . . ?
O2 Pr1 O4 66.34(11) 6 . ?
O2 Pr1 O4 130.23(12) . . ?
O3' Pr1 O4 71.66(12) . . ?
O4 Pr1 O4 132.44(17) 6 . ?
O1 Pr1 Cl1 87.54(8) 6 . ?
O1 Pr1 Cl1 87.54(8) . . ?
O3 Pr1 Cl1 81.6(2) . . ?
O2 Pr1 Cl1 143.86(9) 6 . ?
O2 Pr1 Cl1 143.86(9) . . ?
O3' Pr1 Cl1 97.0(3) . . ?
O4 Pr1 Cl1 77.75(8) 6 . ?
O4 Pr1 Cl1 77.75(8) . . ?
O1 C1 O2 126.0(4) . 2_655 ?
O1 C1 C2 120.7(4) . . ?
O2 C1 C2 113.2(4) 2_655 . ?
N1 C2 C1 112.6(4) . . ?
N1 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
N1 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 N1 108.8(6) 2_755 . ?
N1 C3 H3 125.6 2_755 . ?
N1 C3 H3 125.6 . . ?
N1 C4 C4 101.6(3) . 2_755 ?
N1 C4 H4 129.2 . . ?
C4 C4 H4 129.2 2_755 . ?
C3 N1 C4 114.0(5) . . ?
C3 N1 C2 125.9(4) . . ?
C4 N1 C2 120.1(4) . . ?
C1 O1 Pr1 156.1(3) . . ?
C1 O2 Pr1 135.3(3) 2_655 . ?
C1 O2 H2C 86.3 2_655 . ?
Pr1 O2 H2C 119.9 . . ?
C1 O2 H2D 49.8 2_655 . ?
Pr1 O2 H2D 120.1 . . ?
H2C O2 H2D 120.0 . . ?
Pr1 O4 H4A 121.9 . . ?
Pr1 O4 H4B 132.8 . . ?
H4A O4 H4B 97.1 . . ?
Pr1 O3 H3A 120.0 . . ?
Pr1 O3 H3B 120.0 . . ?
H3A O3 H3B 120.0 . . ?
Pr1 O3 H3'A 173.8 . . ?
H3A O3 H3'A 66.2 . . ?
H3B O3 H3'A 53.8 . . ?
Pr1 O3 H3'B 95.4 . . ?
H3A O3 H3'B 144.6 . . ?
H3B O3 H3'B 24.6 . . ?
H3'A O3 H3'B 78.4 . . ?
Pr1 O3' H3A 94.3 . . ?
Pr1 O3' H3B 174.0 . . ?
H3A O3' H3B 79.7 . . ?
Pr1 O3' H3'A 120.1 . . ?
H3A O3' H3'A 25.9 . . ?
H3B O3' H3'A 53.9 . . ?
Pr1 O3' H3'B 119.9 . . ?
H3A O3' H3'B 145.9 . . ?
H3B O3' H3'B 66.1 . . ?
H3'A O3' H3'B 120.0 . . ?
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 2.425(3) 6 ?
Pr1 O1 2.425(3) . ?
Pr1 O3 2.445(10) . ?
Pr1 O2 2.461(3) 6 ?
Pr1 O2 2.461(3) . ?
Pr1 O3' 2.461(12) . ?
Pr1 O4 2.584(4) 6 ?
Pr1 O4 2.584(4) . ?
Pr1 Cl1 2.7652(17) . ?
C1 O1 1.240(5) . ?
C1 O2 1.270(5) 2_655 ?
C1 C2 1.524(6) . ?
C2 N1 1.475(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.333(5) 2_755 ?
C3 N1 1.333(5) . ?
C3 H3 0.9500 . ?
C4 N1 1.338(7) . ?
C4 C4 1.631(13) 2_755 ?
C4 H4 0.9500 . ?
O2 C1 1.270(5) 2_655 ?
O2 H2C 0.8499 . ?
O2 H2D 0.8501 . ?
O4 H4A 0.8404 . ?
O4 H4B 0.8243 . ?
O3 H3A 0.8500 . ?
O3 H3B 0.8500 . ?
O3 H3'A 0.5373 . ?
O3 H3'B 1.4832 . ?
O3' H3A 1.4761 . ?
O3' H3B 0.5045 . ?
O3' H3'A 0.8500 . ?
O3' H3'B 0.8500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -2.7(6) . . . . ?
O2 C1 C2 N1 177.6(4) 2_655 . . . ?
N1 C3 N1 C4 0.5(4) 2_755 . . . ?
N1 C3 N1 C2 179.3(5) 2_755 . . . ?
C4 C4 N1 C3 -1.1(8) 2_755 . . . ?
C4 C4 N1 C2 -180.0(5) 2_755 . . . ?
C1 C2 N1 C3 55.9(6) . . . . ?
C1 C2 N1 C4 -125.4(5) . . . . ?
O2 C1 O1 Pr1 26.3(11) 2_655 . . . ?
C2 C1 O1 Pr1 -153.4(6) . . . . ?
O1 Pr1 O1 C1 34.0(8) 6 . . . ?
O3 Pr1 O1 C1 -164.9(8) . . . . ?
O2 Pr1 O1 C1 -32.4(8) 6 . . . ?
O2 Pr1 O1 C1 -91.6(8) . . . . ?
O3' Pr1 O1 C1 -139.4(9) . . . . ?
O4 Pr1 O1 C1 -159.9(8) 6 . . . ?
O4 Pr1 O1 C1 57.1(8) . . . . ?
Cl1 Pr1 O1 C1 122.2(8) . . . . ?
O1 Pr1 O2 C1 -14.8(5) 6 . . 2_655 ?
O1 Pr1 O2 C1 48.4(4) . . . 2_655 ?
O3 Pr1 O2 C1 -167.8(5) . . . 2_655 ?
O2 Pr1 O2 C1 -78.7(5) 6 . . 2_655 ?
O3' Pr1 O2 C1 -158.8(5) . . . 2_655 ?
O4 Pr1 O2 C1 125.4(5) 6 . . 2_655 ?
O4 Pr1 O2 C1 -108.1(5) . . . 2_655 ?
Cl1 Pr1 O2 C1 118.5(4) . . . 2_655 ?
