#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:03:52 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179611 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/75/4507547.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_4507547
loop_
_publ_author_name
'Husain, Ahmad'
'Ellwart, Mario'
'Bourne, Susan A.'
'Öhrström Lars'
'Oliver, Clive L.'
_publ_section_title
;
 Single-Crystal-to-Single-Crystal Transformation of a Novel 2-Fold
 Interpenetrated Cadmium-Organic Framework with Trimesate and
 1,2-Bis(4-pyridyl)ethane into the Thermally Desolvated Form Which
 Exhibits Liquid and Gas Sorption Properties
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1526
_journal_paper_doi               10.1021/cg301760a
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C21 H16 Cd N2 O6'
_chemical_formula_sum            'C21 H16 Cd N2 O6'
_chemical_formula_weight         504.76
_chemical_name_common            3
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-02-22 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3913(8)
_cell_length_b                   16.7981(13)
_cell_length_c                   13.8612(11)
_cell_measurement_temperature    173(2)
_cell_volume                     2419.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'X-SEED (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_publication_material  'publCIF (Westrip, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       /w
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9483
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  0.9122
_exptl_absorpt_correction_T_min  0.8348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.141
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2202
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0551
_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)+(0.0736P)²+11.8581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                1883
_reflns_number_total             2202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301760a_si_002.cif
_cod_data_source_block           C:3
_cod_original_sg_symbol_H-M      Pbcm
_cod_database_code               4507547
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -y-1/2, z-1/2'
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_group
Cd1 Cd 1.20380(5) 0.10000(4) 0.2500 0.0297(2) Uani 1 2 d S .
O1 O 1.0690(5) 0.2153(3) 0.2500 0.0372(14) Uani 1 2 d S .
C1 C 0.9710(8) 0.1721(5) 0.2500 0.0310(18) Uani 1 2 d S .
O2 O 0.9787(6) 0.0968(3) 0.2500 0.0405(15) Uani 1 2 d S .
C2 C 0.8435(7) 0.2106(5) 0.2500 0.0339(19) Uani 1 2 d S .
C3 C 0.7290(8) 0.1627(5) 0.2500 0.0369(14) Uani 1 2 d S .
H3 H 0.7364 0.1063 0.2500 0.044 Uiso 1 2 calc SR .
C4 C 0.6081(8) 0.1974(5) 0.2500 0.0369(14) Uani 1 2 d S .
O5 O 0.5765(9) 0.4401(5) 0.2500 0.121(5) Uani 1 2 d SD .
C5 C 0.5984(9) 0.2799(5) 0.2500 0.043(2) Uani 1 2 d S .
H1 H 0.5157 0.3039 0.2500 0.051 Uiso 1 2 calc SR .
O6 O 0.7854(6) 0.4587(4) 0.2500 0.0414(15) Uani 1 2 d S .
C6 C 0.7060(8) 0.3275(5) 0.2500 0.040(2) Uani 1 2 d S .
C7 C 0.8291(8) 0.2926(5) 0.2500 0.0325(18) Uani 1 2 d S .
H7 H 0.9032 0.3257 0.2500 0.039 Uiso 1 2 calc SR .
C8 C 0.6941(10) 0.4168(5) 0.2500 0.047(2) Uani 1 2 d S .
N10 N 1.2126(6) 0.0925(3) 0.0850(4) 0.0460(14) Uani 1 1 d D .
C11 C 1.268(2) 0.0363(11) 0.0324(11) 0.099(8) Uani 0.50 1 d PD -2
H11 H 1.2999 -0.0093 0.0652 0.119 Uiso 0.50 1 calc PR -2
C12 C 1.283(3) 0.0389(14) -0.0649(11) 0.17(2) Uani 0.50 1 d PD -2
H12 H 1.3179 -0.0063 -0.0971 0.210 Uiso 0.50 1 calc PR -2
C13 C 1.2515(18) 0.1031(12) -0.1168(10) 0.072(6) Uani 0.50 1 d PD -2
C14 C 1.181(3) 0.1594(14) -0.0645(12) 0.151(17) Uani 0.50 1 d PD -2
H14 H 1.1374 0.2008 -0.0978 0.181 Uiso 0.50 1 calc PR -2
C15 C 1.174(3) 0.1557(11) 0.0331(11) 0.111(10) Uani 0.50 1 d PD -2
H15 H 1.1403 0.2004 0.0667 0.133 Uiso 0.50 1 calc PR -2
C16 C 1.2714(15) 0.1053(16) -0.2232(9) 0.101(9) Uani 0.50 1 d PD -2
H16A H 1.2987 0.1595 -0.2422 0.121 Uiso 0.50 1 calc PR -2
H16B H 1.3416 0.0681 -0.2404 0.121 Uiso 0.50 1 calc PR -2
C17 C 1.1537(15) 0.0835(10) -0.2784(10) 0.061(5) Uani 0.50 1 d PD -2
H17A H 1.1261 0.0291 -0.2599 0.073 Uiso 0.50 1 calc PR -2
H17B H 1.0833 0.1207 -0.2617 0.073 Uiso 0.50 1 calc PR -2
C18 C 1.1772(18) 0.0862(9) -0.3841(11) 0.054(4) Uani 0.50 1 d PD -2
C19 C 1.107(2) 0.0427(13) -0.4433(11) 0.119(10) Uani 0.50 1 d PD -2
H19 H 1.0392 0.0104 -0.4198 0.143 Uiso 0.50 1 calc PR -2
C20 C 1.136(2) 0.0451(14) -0.5395(10) 0.108(10) Uani 0.50 1 d PD -2
H20 H 1.0930 0.0067 -0.5783 0.130 Uiso 0.50 1 calc PR -2
C21 C 1.298(4) 0.125(3) -0.5326(13) 0.186(16) Uani 0.50 1 d PD -2
H21 H 1.3714 0.1491 -0.5612 0.224 Uiso 0.50 1 calc PR -2
C22 C 1.282(3) 0.126(2) -0.4327(15) 0.186(16) Uani 0.50 1 d PD -2
H22 H 1.3430 0.1545 -0.3947 0.224 Uiso 0.50 1 calc PR -2
C9 C 0.4899(10) 0.1475(6) 0.2500 0.045(2) Uiso 1 2 d S .
O3 O 0.3843(7) 0.1774(4) 0.2500 0.0493(17) Uiso 1 2 d S .
O4 O 0.5106(9) 0.0720(5) 0.2500 0.073(2) Uiso 1 2 d S .
H5A H 0.553(9) 0.488(2) 0.2500 0.05(3) Uiso 1 2 d SD .
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'
Cd Cd -0.8075 1.2024 '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
O3 Cd1 N10 89.90(15) 1_655 6_556
O3 Cd1 N10 89.90(15) 1_655 .
N10 Cd1 N10 172.2(3) 6_556 .
O3 Cd1 O2 146.6(2) 1_655 .
N10 Cd1 O2 92.22(15) 6_556 .
N10 Cd1 O2 92.22(15) . .
O3 Cd1 O6 122.0(2) 1_655 7_755
N10 Cd1 O6 86.76(13) 6_556 7_755
N10 Cd1 O6 86.76(13) . 7_755
O2 Cd1 O6 91.4(2) . 7_755
O3 Cd1 O1 91.2(2) 1_655 .
N10 Cd1 O1 93.88(14) 6_556 .
N10 Cd1 O1 93.88(14) . .
O2 Cd1 O1 55.4(2) . .
O6 Cd1 O1 146.8(2) 7_755 .
O3 Cd1 C1 118.7(3) 1_655 .
N10 Cd1 C1 93.45(15) 6_556 .
N10 Cd1 C1 93.45(15) . .
O2 Cd1 C1 27.9(2) . .
O6 Cd1 C1 119.3(2) 7_755 .
O1 Cd1 C1 27.5(2) . .
C1 O1 Cd1 90.4(5) . .
O1 C1 O2 121.8(7) . .
O1 C1 C2 118.5(7) . .
O2 C1 C2 119.7(8) . .
O1 C1 Cd1 62.1(4) . .
O2 C1 Cd1 59.8(4) . .
C2 C1 Cd1 179.4(6) . .
C1 O2 Cd1 92.3(5) . .
C7 C2 C3 117.9(7) . .
C7 C2 C1 122.3(7) . .
C3 C2 C1 119.8(7) . .
C4 C3 C2 121.0(8) . .
C4 C3 H3 119.5 . .
C2 C3 H3 119.5 . .
C3 C4 C5 119.0(8) . .
C3 C4 C9 120.8(8) . .
C5 C4 C9 120.2(8) . .
C8 O5 H5A 125(7) . .
C6 C5 C4 121.4(8) . .
C6 C5 H1 119.3 . .
C4 C5 H1 119.3 . .
C8 O6 Cd1 129.3(6) . 7_765
C5 C6 C7 119.8(8) . .
C5 C6 C8 120.8(8) . .
C7 C6 C8 119.3(8) . .
C2 C7 C6 120.8(8) . .
C2 C7 H7 119.6 . .
C6 C7 H7 119.6 . .
O6 C8 O5 125.6(9) . .
O6 C8 C6 121.9(9) . .
O5 C8 C6 112.5(9) . .
C21 N10 C20 114.8(14) 6 6
C21 N10 C11 72(2) 6 .
C20 N10 C11 64.1(15) 6 .
C21 N10 C15 64(2) 6 .
C20 N10 C15 92.4(16) 6 .
C11 N10 C15 113.5(11) . .
C21 N10 Cd1 125.1(11) 6 .
C20 N10 Cd1 119.7(8) 6 .
C11 N10 Cd1 127.2(8) . .
C15 N10 Cd1 118.6(8) . .
N10 C11 C12 125.0(16) . .
N10 C11 H11 117.5 . .
C12 C11 H11 117.5 . .
C13 C12 C11 122.1(17) . .
C13 C12 H12 119.0 . .
C11 C12 H12 119.0 . .
C12 C13 C14 113.3(14) . .
C12 C13 C16 121.2(17) . .
C14 C13 C16 124.8(17) . .
C15 C14 C13 121.0(17) . .
C15 C14 H14 119.5 . .
C13 C14 H14 119.5 . .
N10 C15 C14 123.6(15) . .
N10 C15 H15 118.2 . .
C14 C15 H15 118.2 . .
C17 C16 C13 112.9(14) . .
C17 C16 H16A 109.0 . .
C13 C16 H16A 109.0 . .
C17 C16 H16B 109.0 . .
C13 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
C18 C17 C16 111.3(13) . .
C18 C17 H17A 109.4 . .
C16 C17 H17A 109.4 . .
C18 C17 H17B 109.4 . .
C16 C17 H17B 109.4 . .
H17A C17 H17B 108.0 . .
C19 C18 C22 112.5(16) . .
C19 C18 C17 120.5(14) . .
C22 C18 C17 126.7(15) . .
C18 C19 C20 118.3(18) . .
C18 C19 H19 120.9 . .
C20 C19 H19 120.9 . .
N10 C20 C19 128.9(18) 6 .
N10 C20 H20 115.6 6 .
C19 C20 H20 115.6 . .
N10 C21 C22 119(2) 6 .
N10 C21 H21 120.3 6 .
C22 C21 H21 120.3 . .
C21 C22 C18 123(2) . .
C21 C22 H22 118.4 . .
C18 C22 H22 118.4 . .
O3 C9 O4 124.2(10) . .
O3 C9 C4 121.0(9) . .
O4 C9 C4 114.7(9) . .
C9 O3 Cd1 120.7(6) . 1_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O3 2.282(7) 1_655
Cd1 N10 2.293(6) 6_556
Cd1 N10 2.293(6) .
Cd1 O2 2.340(6) .
Cd1 O6 2.375(6) 7_755
Cd1 O1 2.391(6) .
Cd1 C1 2.706(8) .
O1 C1 1.250(10) .
C1 O2 1.267(10) .
C1 C2 1.474(11) .
C2 C7 1.385(11) .
C2 C3 1.437(11) .
C3 C4 1.386(12) .
C3 H3 0.9500 .
C4 C5 1.390(12) .
C4 C9 1.487(13) .
O5 C8 1.283(14) .
O5 H5A 0.84(2) .
C5 C6 1.374(12) .
C5 H1 0.9500 .
O6 C8 1.182(11) .
O6 Cd1 2.375(6) 7_765
C6 C7 1.407(12) .
C6 C8 1.505(12) .
C7 H7 0.9500 .
N10 C21 1.27(2) 6
N10 C20 1.292(18) 6
N10 C11 1.327(14) .
N10 C15 1.343(14) .
C11 C12 1.358(16) .
C11 H11 0.9500 .
C12 C13 1.340(17) .
C12 H12 0.9500 .
C13 C14 1.398(17) .
C13 C16 1.489(15) .
C14 C15 1.356(16) .
C14 H14 0.9500 .
C15 H15 0.9500 .
C16 C17 1.488(15) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.49(2) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 C19 1.317(17) .
C18 C22 1.446(17) .
C19 C20 1.366(16) .
C19 H19 0.9500 .
C20 N10 1.292(18) 6
C20 H20 0.9500 .
C21 N10 1.27(2) 6
C21 C22 1.394(18) .
C21 H21 0.9500 .
C22 H22 0.9500 .
C9 O3 1.207(11) .
C9 O4 1.286(13) .
O3 Cd1 2.282(7) 1_455
