#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:45:27 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180447 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/16/7211616.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_7211616
loop_
_publ_author_name
'Wang, Dengxu'
'He, Haiyan'
'Chen, Xiaohui'
'Feng, Shengyu'
'Niu, Yuzhong'
'Sun, Daofeng'
_publ_section_title
;
 A 3D porous metal--organic framework constructed of 1D zigzag and helical
 chains exhibiting selective anion exchange
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              1041
_journal_paper_doi               10.1039/b910988a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C20 H21.52 N4 O1.52 Si'
_chemical_formula_weight         371.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.772(2)
_cell_length_b                   19.128(7)
_cell_length_c                   17.295(6)
_cell_measurement_reflns_used    3503
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.71
_cell_measurement_theta_min      2.17
_cell_volume                     1909.5(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0764
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10565
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_correction_T_min  0.9790
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.001(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0694
_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)+(0.1138P)²+0.3779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2222
_reflns_number_gt                1236
_reflns_number_total             2263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910988a.txt
_cod_data_source_block           d:\bips\bips
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7211616
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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
Si1 Si 0.0733(2) 0.7500 0.42035(7) 0.0453(4) Uani 1 2 d S
N1 N 0.7037(5) 0.49770(13) 0.37601(15) 0.0509(8) Uani 1 1 d .
N2 N 1.0169(7) 0.4325(2) 0.3818(2) 0.0928(13) Uani 1 1 d .
C1 C 0.2590(5) 0.67064(16) 0.40730(17) 0.0427(8) Uani 1 1 d .
C2 C 0.4003(6) 0.64591(17) 0.46662(19) 0.0502(8) Uani 1 1 d .
H2A H 0.3970 0.6684 0.5143 0.060 Uiso 1 1 calc R
C3 C 0.5451(6) 0.58909(17) 0.45703(19) 0.0497(8) Uani 1 1 d .
H3A H 0.6372 0.5737 0.4978 0.060 Uiso 1 1 calc R
C4 C 0.5522(5) 0.55547(17) 0.38699(18) 0.0460(8) Uani 1 1 d .
C5 C 0.4151(6) 0.57785(16) 0.32695(18) 0.0492(8) Uani 1 1 d .
H5A H 0.4192 0.5549 0.2796 0.059 Uiso 1 1 calc R
C6 C 0.2710(6) 0.63481(16) 0.33753(18) 0.0473(8) Uani 1 1 d .
H6A H 0.1791 0.6497 0.2965 0.057 Uiso 1 1 calc R
C7 C 0.6579(8) 0.4370(2) 0.3372(2) 0.0689(11) Uani 1 1 d .
C8 C 0.8433(9) 0.3974(2) 0.3406(2) 0.0760(13) Uani 1 1 d .
H8 H 0.8574 0.3531 0.3190 0.091 Uiso 1 1 calc R
C9 C 0.9254(7) 0.4924(2) 0.4016(2) 0.0636(10) Uani 1 1 d .
C10 C -0.0465(9) 0.7500 0.5204(3) 0.0621(14) Uani 1 2 d S
H10A H -0.1419 0.7906 0.5276 0.093 Uiso 0.50 1 calc PR
H10B H 0.0785 0.7507 0.5570 0.093 Uiso 1 2 calc SR
H10C H -0.1379 0.7087 0.5281 0.093 Uiso 0.50 1 calc PR
C11 C -0.1555(8) 0.7500 0.3465(3) 0.0572(13) Uani 1 2 d S
H11A H -0.0863 0.7500 0.2960 0.086 Uiso 1 2 calc SR
H11B H -0.2499 0.7910 0.3524 0.086 Uiso 0.50 1 calc PR
H11C H -0.2499 0.7090 0.3524 0.086 Uiso 0.50 1 calc PR
H9 H 0.9956 0.5316 0.4304 0.085(13) Uiso 1 1 d R
H7 H 0.5077 0.4277 0.3058 0.116(16) Uiso 1 1 d R
O01 O 0.899(5) 0.2500 0.2152(15) 0.64(4) Uiso 1.51(13) 2 d SP
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'
Si Si 0.0817 0.0704 '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
C11 Si1 C10 112.3(2) . .
C11 Si1 C1 109.12(13) . 8_575
C10 Si1 C1 108.94(13) . 8_575
C11 Si1 C1 109.12(13) . .
C10 Si1 C1 108.94(13) . .
C1 Si1 C1 108.38(19) 8_575 .
C9 N1 C7 106.2(3) . .
C9 N1 C4 126.4(3) . .
C7 N1 C4 127.4(3) . .
C9 N2 C8 105.3(4) . .
C6 C1 C2 116.3(3) . .
C6 C1 Si1 122.2(2) . .
C2 C1 Si1 121.4(2) . .
C3 C2 C1 122.2(3) . .
C3 C2 H2A 118.9 . .
C1 C2 H2A 118.9 . .
C4 C3 C2 119.5(3) . .
C4 C3 H3A 120.2 . .
C2 C3 H3A 120.2 . .
C5 C4 C3 120.3(3) . .
C5 C4 N1 119.7(3) . .
C3 C4 N1 120.0(3) . .
C4 C5 C6 119.5(3) . .
C4 C5 H5A 120.3 . .
C6 C5 H5A 120.3 . .
C5 C6 C1 122.2(3) . .
C5 C6 H6A 118.9 . .
C1 C6 H6A 118.9 . .
C8 C7 N1 108.1(4) . .
C8 C7 H7 127.2 . .
N1 C7 H7 124.3 . .
C7 C8 N2 109.2(4) . .
C7 C8 H8 125.4 . .
N2 C8 H8 125.4 . .
N2 C9 N1 111.2(4) . .
N2 C9 H9 129.2 . .
N1 C9 H9 119.6 . .
Si1 C10 H10A 109.5 . .
Si1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Si1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Si1 C11 H11A 109.5 . .
Si1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
Si1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C11 1.838(5) .
Si1 C10 1.863(5) .
Si1 C1 1.872(3) 8_575
Si1 C1 1.872(3) .
N1 C9 1.358(5) .
N1 C7 1.367(4) .
N1 C4 1.422(4) .
N2 C9 1.306(5) .
N2 C8 1.401(6) .
C1 C6 1.390(4) .
C1 C2 1.394(4) .
C2 C3 1.381(5) .
C2 H2A 0.9300 .
C3 C4 1.372(4) .
C3 H3A 0.9300 .
C4 C5 1.374(4) .
C5 C6 1.383(4) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
C7 C8 1.312(5) .
C7 H7 1.0390 .
C8 H8 0.9300 .
C9 H9 0.9873 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
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
C11 Si1 C1 C6 21.7(3) .
C10 Si1 C1 C6 144.6(3) .
C1 Si1 C1 C6 -97.0(3) 8_575
C11 Si1 C1 C2 -160.9(3) .
C10 Si1 C1 C2 -38.0(3) .
C1 Si1 C1 C2 80.4(3) 8_575
C6 C1 C2 C3 0.1(5) .
Si1 C1 C2 C3 -177.4(3) .
C1 C2 C3 C4 0.2(5) .
C2 C3 C4 C5 -0.4(5) .
C2 C3 C4 N1 178.9(3) .
C9 N1 C4 C5 137.8(4) .
C7 N1 C4 C5 -41.4(5) .
C9 N1 C4 C3 -41.5(5) .
C7 N1 C4 C3 139.3(4) .
C3 C4 C5 C6 0.4(5) .
N1 C4 C5 C6 -178.9(3) .
C4 C5 C6 C1 -0.1(5) .
C2 C1 C6 C5 -0.1(5) .
Si1 C1 C6 C5 177.4(2) .
C9 N1 C7 C8 0.7(4) .
C4 N1 C7 C8 -180.0(3) .
N1 C7 C8 N2 -0.5(5) .
C9 N2 C8 C7 0.0(5) .
C8 N2 C9 N1 0.4(5) .
C7 N1 C9 N2 -0.7(4) .
C4 N1 C9 N2 180.0(3) .
