#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/92/4309216.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_4309216
loop_
_publ_author_name
'Bao-Qing Ma'
'Karen L. Mulfort'
'Joseph T. Hupp'
_publ_section_title
;
Microporous Pillared Paddle-Wheel Frameworks Based on Mixed-Ligand
Coordination of Zinc Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4912
_journal_page_last               4914
_journal_paper_doi               10.1021/ic050452i
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C19.5 H15.5 N2.5 O8.5 Zn2'
_chemical_formula_weight         551.58
_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                 105.407(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4458(17)
_cell_length_b                   11.5837(15)
_cell_length_c                   14.0404(18)
_cell_measurement_temperature    120(1)
_cell_volume                     2108.2(5)
_computing_cell_refinement       SMART
_computing_data_collection       smart
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'SMART CCD 1000'
_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  0.1693
_diffrn_reflns_av_sigmaI/netI    0.1213
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10298
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    2.330
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   'face index'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.114
_refine_diff_density_min         -2.386
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0740
_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)+(0.1049P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1793
_refine_ls_wR_factor_ref         0.2104
_reflns_number_gt                1901
_reflns_number_total             2766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050452isi20050325_110047.cif
_cod_data_source_block           c2m
_cod_original_formula_sum        'C19.50 H15.50 N2.50 O8.50 Zn2'
_cod_database_code               4309216
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
Zn1 Zn 0.73846(6) 0.5000 0.58264(6) 0.0126(3) Uani 1 2 d S . .
Zn2 Zn 0.76892(6) 0.5000 0.79925(6) 0.0129(3) Uani 1 2 d S . .
N1 N 0.7406(5) 0.5000 0.4388(5) 0.0187(14) Uani 1 2 d S . .
N2 N 0.7755(6) 0.5000 -0.0546(5) 0.0245(15) Uani 1 2 d S . .
O1 O 0.8500(3) 0.3779(4) 0.6322(3) 0.0353(11) Uani 1 1 d . . .
O2 O 0.8769(4) 0.3788(4) 0.7958(3) 0.0449(13) Uani 1 1 d . . .
O3 O 1.1568(4) 0.1214(4) 0.7526(3) 0.0376(12) Uani 1 1 d . . .
O4 O 1.1315(3) 0.1215(4) 0.5884(3) 0.0340(11) Uani 1 1 d . . .
C1 C 0.8971(5) 0.3467(5) 0.7164(5) 0.0278(14) Uani 1 1 d . . .
C2 C 0.9865(5) 0.2671(6) 0.7283(5) 0.0367(17) Uani 1 1 d . . .
H2A H 1.0221 0.2435 0.7932 0.044 Uiso 1 1 calc R . .
C3 C 1.0186(5) 0.2280(6) 0.6547(5) 0.0318(15) Uani 1 1 d . . .
H3A H 0.9818 0.2501 0.5898 0.038 Uiso 1 1 calc R . .
C4 C 1.1098(5) 0.1504(5) 0.6663(5) 0.0298(14) Uani 1 1 d . . .
C5 C 0.7452(5) 0.5985(5) 0.3911(5) 0.0344(16) Uani 1 1 d . . .
H5A H 0.7439 0.6694 0.4246 0.041 Uiso 1 1 calc R . .
C6 C 0.7519(5) 0.6011(5) 0.2943(4) 0.0366(18) Uani 1 1 d . . .
H6A H 0.7528 0.6728 0.2617 0.044 Uiso 1 1 calc R . .
C7 C 0.7570(6) 0.5000 0.2460(6) 0.0239(18) Uani 1 2 d S . .
C8 C 0.7657(7) 0.5000 0.1411(6) 0.0247(18) Uani 1 2 d S . .
C9 C 0.7681(17) 0.5924(10) 0.0923(8) 0.233(12) Uani 1 1 d . . .
H9A H 0.7664 0.6655 0.1226 0.280 Uiso 1 1 calc R . .
C10 C 0.7730(17) 0.5858(10) -0.0063(9) 0.219(10) Uani 1 1 d . . .
H10A H 0.7746 0.6574 -0.0389 0.262 Uiso 1 1 calc R . .
O6 O 0.9938(17) 0.0534(18) 1.0647(16) 0.260(13) Uiso 0.25 1 d P . .
C12 C 0.9938(17) 0.0534(18) 1.0647(16) 0.260(13) Uiso 0.50 1 d P . .
C11 C 1.0000 0.269(3) 1.0000 0.072(8) Uiso 0.50 2 d SP . .
N3 N 1.0000 0.159(3) 1.0000 0.143(13) Uiso 0.50 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'
Zn Zn 0.2839 1.4301 '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
N1 Zn1 O4 103.75(18) . 8_455 ?
N1 Zn1 O4 103.75(17) . 3_455 ?
O4 Zn1 O4 87.8(3) 8_455 3_455 ?
N1 Zn1 O1 97.79(18) . 6_565 ?
O4 Zn1 O1 158.42(18) 8_455 6_565 ?
O4 Zn1 O1 88.3(2) 3_455 6_565 ?
N1 Zn1 O1 97.79(18) . . ?
O4 Zn1 O1 88.3(2) 8_455 . ?
O4 Zn1 O1 158.42(18) 3_455 . ?
O1 Zn1 O1 87.5(3) 6_565 . ?
N1 Zn1 Zn2 171.53(18) . . ?
O4 Zn1 Zn2 82.24(12) 8_455 . ?
O4 Zn1 Zn2 82.24(12) 3_455 . ?
O1 Zn1 Zn2 76.20(13) 6_565 . ?
O1 Zn1 Zn2 76.20(13) . . ?
O2 Zn2 O2 87.6(3) 6_565 . ?
O2 Zn2 N2 100.6(2) 6_565 1_556 ?
O2 Zn2 N2 100.6(2) . 1_556 ?
O2 Zn2 O3 160.45(19) 6_565 8_455 ?
O2 Zn2 O3 89.3(2) . 8_455 ?
N2 Zn2 O3 98.92(19) 1_556 8_455 ?
O2 Zn2 O3 89.3(2) 6_565 3_455 ?
O2 Zn2 O3 160.45(19) . 3_455 ?
N2 Zn2 O3 98.92(19) 1_556 3_455 ?
O3 Zn2 O3 87.3(3) 8_455 3_455 ?
O2 Zn2 Zn1 83.12(13) 6_565 . ?
O2 Zn2 Zn1 83.12(13) . . ?
N2 Zn2 Zn1 174.7(2) 1_556 . ?
O3 Zn2 Zn1 77.34(12) 8_455 . ?
O3 Zn2 Zn1 77.34(12) 3_455 . ?
C5 N1 C5 117.7(8) . 6_565 ?
C5 N1 Zn1 121.0(4) . . ?
C5 N1 Zn1 121.0(4) 6_565 . ?
C10 N2 C10 110.7(12) . 6_565 ?
C10 N2 Zn2 124.5(6) . 1_554 ?
C10 N2 Zn2 124.5(6) 6_565 1_554 ?
C1 O1 Zn1 132.1(4) . . ?
C1 O2 Zn2 123.0(4) . . ?
C4 O3 Zn2 129.4(4) . 3_545 ?
C4 O4 Zn1 123.6(4) . 3_545 ?
O1 C1 O2 125.3(5) . . ?
O1 C1 C2 118.8(5) . . ?
O2 C1 C2 115.9(5) . . ?
C3 C2 C1 123.6(6) . . ?
C2 C3 C4 123.9(6) . . ?
O4 C4 O3 126.8(5) . . ?
O4 C4 C3 116.2(6) . . ?
O3 C4 C3 117.1(5) . . ?
N1 C5 C6 122.4(6) . . ?
C7 C6 C5 119.6(6) . . ?
C6 C7 C6 118.3(8) . 6_565 ?
C6 C7 C8 120.8(4) . . ?
C6 C7 C8 120.8(4) 6_565 . ?
C9 C8 C9 114.1(11) 6_565 . ?
C9 C8 C7 122.9(5) 6_565 . ?
C9 C8 C7 122.9(5) . . ?
C8 C9 C10 119.8(11) . . ?
N2 C10 C9 127.8(11) . . ?
N2 C10 C10 34.7(6) . 6_565 ?
C9 C10 C10 93.1(7) . 6_565 ?
C12 O6 O6 0.000(7) 6 6 ?
C12 O6 N3 142.8(12) 6 . ?
O6 O6 N3 142.8(12) 6 . ?
C12 O6 C12 90.000(5) 6 2_757 ?
O6 O6 C12 90.000(5) 6 2_757 ?
N3 O6 C12 52.8(12) . 2_757 ?
C11 N3 C12 142.8(12) . 2_757 ?
C11 N3 O6 142.8(12) . 2_757 ?
C12 N3 O6 0.0(10) 2_757 2_757 ?
C11 N3 O6 142.8(12) . . ?
C12 N3 O6 74(2) 2_757 . ?
O6 N3 O6 74(2) 2_757 . ?
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
Zn1 N1 2.028(7) . ?
Zn1 O4 2.029(4) 8_455 ?
Zn1 O4 2.029(4) 3_455 ?
Zn1 O1 2.045(4) 6_565 ?
Zn1 O1 2.045(4) . ?
Zn1 Zn2 2.9589(12) . ?
Zn2 O2 2.029(4) 6_565 ?
Zn2 O2 2.029(4) . ?
Zn2 N2 2.031(7) 1_556 ?
Zn2 O3 2.038(4) 8_455 ?
Zn2 O3 2.038(4) 3_455 ?
N1 C5 1.332(7) . ?
N1 C5 1.332(6) 6_565 ?
N2 C10 1.208(10) . ?
N2 C10 1.208(10) 6_565 ?
N2 Zn2 2.031(7) 1_554 ?
O1 C1 1.237(7) . ?
O2 C1 1.272(7) . ?
O3 C4 1.254(7) . ?
O3 Zn2 2.038(4) 3_545 ?
O4 C4 1.251(7) . ?
O4 Zn1 2.029(4) 3_545 ?
C1 C2 1.488(7) . ?
C2 C3 1.302(9) . ?
C3 C4 1.494(7) . ?
C5 C6 1.386(7) . ?
C6 C7 1.363(7) . ?
C7 C6 1.363(7) 6_565 ?
C7 C8 1.508(11) . ?
C8 C9 1.276(11) 6_565 ?
C8 C9 1.276(11) . ?
C9 C10 1.407(12) . ?
C10 C10 1.99(2) 6_565 ?
O6 C12 1.24(4) 6 ?
O6 O6 1.24(4) 6 ?
O6 N3 1.54(3) . ?
O6 C12 1.87(4) 2_757 ?
C11 N3 1.27(4) . ?
N3 C12 1.54(3) 2_757 ?
N3 O6 1.54(3) 2_757 ?
