#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:32:58 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179850 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/46/7014623.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_7014623
loop_
_publ_author_name
'Willans, Charlotte E.'
'French, Sara'
'Anderson, Kirsty M.'
'Barbour, Leonard J.'
'Gertenbach, Jan-André'
'Lloyd, Gareth O.'
'Dyer, Robert J.'
'Junk, Peter C.'
'Steed, Jonathan W.'
_publ_section_title
;
 Tripodal imidazole frameworks: Reversible vapour sorption both with
 and without significant structural changes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              573
_journal_page_last               582
_journal_paper_doi               10.1039/c0dt01011a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C24 H30 Cd Cl2 N6'
_chemical_formula_weight         585.84
_chemical_name_common            'Cd Complex'
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2n'
_symmetry_space_group_name_H-M   'P n a m'
_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                   9.1574(12)
_cell_length_b                   21.172(3)
_cell_length_c                   12.8437(15)
_cell_measurement_temperature    120(2)
_cell_volume                     2490.1(6)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    X-SEED
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'SMART 1K'
_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  0.1492
_diffrn_reflns_av_sigmaI/netI    0.2171
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10792
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  0.8966
_exptl_absorpt_correction_T_min  0.8076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.764
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.764
_refine_ls_R_factor_all          0.1525
_refine_ls_R_factor_gt           0.0581
_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)+(0.0095P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                1252
_reflns_number_total             2931
_reflns_threshold_expression     >2s(I)
_cod_data_source_file            C0DT01011A.TXT
_cod_data_source_block           PNA21.CIF
_cod_original_cell_volume        2490.2(5)
_cod_original_sg_symbol_H-M      Pnam
_cod_database_code               7014623
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'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
Cd1 Cd 0.43135(8) 0.61430(4) 0.2500 0.0356(2) Uani 1 2 d S . .
Cl1 Cl 0.4910(3) 0.49409(11) 0.2500 0.0372(6) Uani 1 2 d S . .
Cl2 Cl 0.3696(3) 0.73149(12) 0.2500 0.0570(8) Uani 1 2 d S . .
N12 N 0.4332(7) 0.3708(3) -0.1034(4) 0.0467(16) Uani 1 1 d . . .
N15 N -0.0145(10) 0.5306(4) 0.2500 0.047(2) Uani 1 2 d S . .
N19 N 0.1887(9) 0.5882(4) 0.2500 0.040(2) Uani 1 2 d S . .
N24 N 0.2707(6) 0.3381(3) 0.0115(4) 0.0388(16) Uani 1 1 d . . .
C1 C 0.1324(13) 0.5301(5) 0.2500 0.051(3) Uani 1 2 d S . .
H1 H 0.1895 0.4926 0.2500 0.061 Uiso 1 2 calc SR . .
C2 C 0.0698(13) 0.6279(5) 0.2500 0.046(3) Uani 1 2 d S . .
H2 H 0.0741 0.6727 0.2500 0.055 Uiso 1 2 calc SR . .
C3 C -0.0562(14) 0.5926(5) 0.2500 0.058(3) Uani 1 2 d S . .
H3 H -0.1535 0.6083 0.2500 0.069 Uiso 1 2 calc SR . .
C4 C -0.1150(12) 0.4751(5) 0.2500 0.059(3) Uani 1 2 d S . .
H4A H -0.1784 0.4769 0.1876 0.071 Uiso 0.50 1 calc PR . .
H4B H -0.1784 0.4769 0.3124 0.071 Uiso 0.50 1 calc PR . .
C5 C -0.0315(10) 0.4138(4) 0.2500 0.034(3) Uani 1 2 d S . .
C6 C 0.0117(7) 0.3860(4) 0.1544(5) 0.0421(19) Uani 1 1 d . . .
C7 C -0.0355(8) 0.4172(4) 0.0533(5) 0.063(3) Uani 1 1 d . . .
H7A H -0.0339 0.4636 0.0619 0.076 Uiso 1 1 calc R . .
H7B H 0.0345 0.4060 -0.0025 0.076 Uiso 1 1 calc R . .
C8 C -0.1878(10) 0.3964(5) 0.0215(5) 0.109(4) Uani 1 1 d . . .
H8A H -0.1864 0.3514 0.0035 0.164 Uiso 1 1 calc R . .
H8B H -0.2198 0.4210 -0.0390 0.164 Uiso 1 1 calc R . .
H8C H -0.2555 0.4033 0.0795 0.164 Uiso 1 1 calc R . .
C9 C 0.0928(8) 0.3308(3) 0.1550(5) 0.0355(18) Uani 1 1 d . . .
C10 C 0.1440(8) 0.3037(3) 0.0525(5) 0.052(2) Uani 1 1 d . . .
H10A H 0.1703 0.2588 0.0623 0.063 Uiso 1 1 calc R . .
H10B H 0.0633 0.3058 0.0013 0.063 Uiso 1 1 calc R . .
C11 C 0.3365(8) 0.3281(4) -0.0812(5) 0.045(2) Uani 1 1 d . . .
H11 H 0.3143 0.2934 -0.1254 0.054 Uiso 1 1 calc R . .
C12 C 0.4363(9) 0.4112(3) -0.0185(6) 0.060(2) Uani 1 1 d . . .
H12 H 0.4965 0.4475 -0.0116 0.072 Uiso 1 1 calc R . .
C13 C 0.3390(8) 0.3901(4) 0.0531(6) 0.060(2) Uani 1 1 d . . .
H13 H 0.3213 0.4080 0.1198 0.072 Uiso 1 1 calc R . .
C14 C 0.1347(11) 0.3055(5) 0.2500 0.042(3) Uani 1 2 d S . .
C15 C 0.2253(12) 0.2426(5) 0.2500 0.059(3) Uani 1 2 d S . .
H15A H 0.2887 0.2413 0.1876 0.071 Uiso 0.50 1 calc PR . .
H15B H 0.2887 0.2413 0.3124 0.071 Uiso 0.50 1 calc PR . .
C16 C 0.1225(12) 0.1846(5) 0.2500 0.061(3) Uani 1 2 d S . .
H16A H 0.1808 0.1458 0.2500 0.091 Uiso 1 2 calc SR . .
H16B H 0.0607 0.1856 0.1877 0.091 Uiso 0.50 1 calc PR . .
H16C H 0.0607 0.1856 0.3123 0.091 Uiso 0.50 1 calc PR . .
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'
Cd Cd -0.8075 1.2024 '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'
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
N12 Cd1 N12 111.6(3) 2_665 5_665 ?
N12 Cd1 N19 124.21(15) 2_665 . ?
N12 Cd1 N19 124.21(15) 5_665 . ?
N12 Cd1 Cl2 89.20(15) 2_665 . ?
N12 Cd1 Cl2 89.20(15) 5_665 . ?
N19 Cd1 Cl2 91.1(2) . . ?
N12 Cd1 Cl1 91.21(15) 2_665 . ?
N12 Cd1 Cl1 91.21(15) 5_665 . ?
N19 Cd1 Cl1 88.2(2) . . ?
Cl2 Cd1 Cl1 179.27(9) . . ?
C11 N12 C12 105.7(6) . . ?
C11 N12 Cd1 130.6(5) . 5_665 ?
C12 N12 Cd1 123.6(5) . 5_665 ?
C1 N15 C3 106.7(10) . . ?
C1 N15 C4 127.6(10) . . ?
C3 N15 C4 125.7(10) . . ?
C1 N19 C2 104.9(9) . . ?
C1 N19 Cd1 126.7(8) . . ?
C2 N19 Cd1 128.4(7) . . ?
C11 N24 C13 105.4(6) . . ?
C11 N24 C10 126.2(6) . . ?
C13 N24 C10 128.2(6) . . ?
N19 C1 N15 112.2(10) . . ?
N19 C2 C3 109.4(9) . . ?
N15 C3 C2 106.7(10) . . ?
N15 C4 C5 111.4(9) . . ?
C6 C5 C6 119.9(9) . 6_556 ?
C6 C5 C4 120.0(5) . . ?
C6 C5 C4 120.0(5) 6_556 . ?
C9 C6 C5 119.7(7) . . ?
C9 C6 C7 121.5(6) . . ?
C5 C6 C7 118.7(7) . . ?
C8 C7 C6 111.4(6) . . ?
C6 C9 C14 118.6(7) . . ?
C6 C9 C10 118.9(6) . . ?
C14 C9 C10 122.3(7) . . ?
N24 C10 C9 111.7(5) . . ?
N12 C11 N24 112.8(6) . . ?
C13 C12 N12 108.5(7) . . ?
C12 C13 N24 107.4(7) . . ?
C9 C14 C9 123.3(10) . 6_556 ?
C9 C14 C15 118.3(5) . . ?
C9 C14 C15 118.3(5) 6_556 . ?
C16 C15 C14 110.6(9) . . ?
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
Cd1 N12 2.277(6) 2_665 ?
Cd1 N12 2.277(6) 5_665 ?
Cd1 N19 2.290(8) . ?
Cd1 Cl2 2.545(3) . ?
Cd1 Cl1 2.603(2) . ?
N12 C11 1.298(8) . ?
N12 C12 1.386(7) . ?
N12 Cd1 2.277(6) 5_665 ?
N15 C1 1.345(11) . ?
N15 C3 1.367(11) . ?
N15 C4 1.493(12) . ?
N19 C1 1.335(12) . ?
N19 C2 1.375(12) . ?
N24 C11 1.351(7) . ?
N24 C13 1.374(8) . ?
N24 C10 1.468(8) . ?
C2 C3 1.375(14) . ?
C4 C5 1.506(12) . ?
C5 C6 1.418(8) . ?
C5 C6 1.418(8) 6_556 ?
C6 C9 1.384(9) . ?
C6 C7 1.520(8) . ?
C7 C8 1.518(9) . ?
C9 C14 1.387(8) . ?
C9 C10 1.510(8) . ?
C12 C13 1.356(9) . ?
C14 C9 1.387(8) 6_556 ?
C14 C15 1.570(13) . ?
C15 C16 1.548(12) . ?
