#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:17:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180421 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/90/7209010.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_7209010
loop_
_publ_author_name
'Jacobs, Tia'
'Barbour, Leonard J.'
_publ_section_title
;
 Solvent diffusion and binding in a ‘nonporous’ molecular
 crystal
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1512
_journal_paper_doi               10.1039/c2ce26404h
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C44 H44 Cd2 I4 N8, C H2 Cl2'
_chemical_formula_sum            'C45 H46 Cd2 Cl2 I4 N8'
_chemical_formula_weight         1502.20
_chemical_name_common            3_CH2Cl2
_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                 113.843(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.799(2)
_cell_length_b                   16.188(2)
_cell_length_c                   9.4162(12)
_cell_measurement_reflns_used    4334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.37
_cell_volume                     2481.5(5)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
X-Seed (Barbour, 2001; Atwood & Barbour, 2003)
;
_computing_publication_material
;
X-Seed (Atwood & Barbour, 2003; Barbour, 2001)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6979
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.493
_exptl_absorpt_correction_T_max  0.5529
_exptl_absorpt_correction_T_min  0.3860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.525
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0311
_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)+(0.0209P)²+41.3318P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                2262
_reflns_number_total             2547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26404h.txt
_cod_data_source_block           5
_cod_original_cell_volume        2481.6(5)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7209010
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
Cd1 Cd 0.23082(3) 0.0000 0.41649(6) 0.01973(15) Uani 1 2 d S . 1
I2 I 0.39878(3) 0.0000 0.55072(6) 0.02371(15) Uani 1 2 d S . 1
I3 I 0.16985(4) 0.0000 0.09909(6) 0.02914(16) Uani 1 2 d S . 1
C14 C 0.0270(3) 0.2886(3) 0.9563(6) 0.0165(11) Uani 1 1 d . . 1
C10 C 0.1911(4) 0.2942(4) 0.7208(7) 0.0256(13) Uani 1 1 d . . 1
H10A H 0.1865 0.3488 0.6708 0.031 Uiso 1 1 calc R . 1
H10B H 0.2479 0.2885 0.8003 0.031 Uiso 1 1 calc R . 1
C8 C 0.2152(3) 0.1566(4) 0.6190(6) 0.0217(12) Uani 1 1 d . . 1
C16 C 0.1199(3) 0.2183(4) 0.8676(6) 0.0226(12) Uani 1 1 d . . 1
H16 H 0.1473 0.1692 0.8605 0.027 Uiso 1 1 calc R . 1
C9 C 0.2824(4) 0.1264(4) 0.7627(7) 0.0349(15) Uani 1 1 d . . 1
H9A H 0.3106 0.1736 0.8275 0.052 Uiso 1 1 calc R . 1
H9B H 0.3216 0.0945 0.7358 0.052 Uiso 1 1 calc R . 1
H9C H 0.2595 0.0912 0.8200 0.052 Uiso 1 1 calc R . 1
C15 C 0.0683(3) 0.2176(3) 0.9449(6) 0.0197(11) Uani 1 1 d . . 1
H15 H 0.0609 0.1678 0.9911 0.024 Uiso 1 1 calc R . 1
N7 N 0.1760(3) 0.2293(3) 0.6029(5) 0.0225(10) Uani 1 1 d . . 1
N4 N 0.1847(3) 0.1157(3) 0.4842(5) 0.0261(11) Uani 1 1 d . . 1
C11 C 0.1317(3) 0.2907(3) 0.8002(6) 0.0199(11) Uani 1 1 d . . 1
C12 C 0.0902(3) 0.3613(3) 0.8091(6) 0.0199(11) Uani 1 1 d . . 1
H12 H 0.0972 0.4108 0.7616 0.024 Uiso 1 1 calc R . 1
C5 C 0.1250(4) 0.1652(5) 0.3827(7) 0.0372(16) Uani 1 1 d . . 1
H5 H 0.0931 0.1523 0.2769 0.045 Uiso 1 1 calc R . 1
C13 C 0.0385(3) 0.3607(4) 0.8863(6) 0.0220(12) Uani 1 1 d . . 1
H13 H 0.0106 0.4099 0.8917 0.026 Uiso 1 1 calc R . 1
Cl18 Cl -0.0459(13) -0.0106(14) 0.3322(12) 0.026(3) Uiso 0.13 1 d PD A -1
C6 C 0.1180(4) 0.2347(4) 0.4539(7) 0.0330(15) Uani 1 1 d . . 1
H6 H 0.0804 0.2786 0.4098 0.040 Uiso 1 1 calc R . 1
Cl21 Cl -0.0110(9) -0.0072(19) 0.3224(12) 0.035(3) Uiso 0.13 1 d PD B -2
C17 C -0.001(3) 0.0481(15) 0.509(3) 0.005(7) Uiso 0.13 1 d PD A -1
H17A H 0.0252 0.0983 0.4909 0.006 Uiso 0.13 1 calc PR A -1
H17B H -0.0451 0.0655 0.5423 0.006 Uiso 0.13 1 calc PR A -1
C20 C -0.026(5) -0.026(5) 0.495(5) 0.11(4) Uiso 0.13 1 d PD B -2
H20A H -0.0195 -0.0857 0.5207 0.128 Uiso 0.13 1 calc PR B -2
H20B H -0.0815 -0.0086 0.4817 0.128 Uiso 0.13 1 calc PR B -2
Cl19 Cl 0.0729(8) -0.0132(9) 0.6579(11) 0.018(3) Uiso 0.13 1 d PD A -1
Cl22 Cl 0.050(4) 0.032(3) 0.647(5) 0.16(2) Uiso 0.13 1 d PD B -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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
N4 Cd1 N4 113.6(3) 6 .
N4 Cd1 I2 109.06(13) 6 .
N4 Cd1 I2 109.06(13) . .
N4 Cd1 I3 106.37(12) 6 .
N4 Cd1 I3 106.37(12) . .
I2 Cd1 I3 112.43(3) . .
C15 C14 C13 118.2(5) . .
C15 C14 C14 121.2(3) . 2_557
C13 C14 C14 120.6(3) . 2_557
N7 C10 C11 113.2(5) . .
N7 C10 H10A 108.9 . .
C11 C10 H10A 108.9 . .
N7 C10 H10B 108.9 . .
C11 C10 H10B 108.9 . .
H10A C10 H10B 107.8 . .
N4 C8 N7 109.5(5) . .
N4 C8 C9 124.9(5) . .
N7 C8 C9 125.6(5) . .
C15 C16 C11 120.2(5) . .
C15 C16 H16 119.9 . .
C11 C16 H16 119.9 . .
C16 C15 C14 121.1(5) . .
C16 C15 H15 119.4 . .
C14 C15 H15 119.4 . .
C8 N7 C6 108.3(5) . .
C8 N7 C10 127.7(5) . .
C6 N7 C10 124.1(5) . .
C8 N4 C5 106.0(5) . .
C8 N4 Cd1 129.1(4) . .
C5 N4 Cd1 124.3(4) . .
C12 C11 C16 119.2(5) . .
C12 C11 C10 119.6(5) . .
C16 C11 C10 121.2(5) . .
C11 C12 C13 120.7(5) . .
C11 C12 H12 119.6 . .
C13 C12 H12 119.6 . .
C6 C5 N4 110.3(6) . .
C6 C5 H5 124.9 . .
N4 C5 H5 124.9 . .
C12 C13 C14 120.6(5) . .
C12 C13 H13 119.7 . .
C14 C13 H13 119.7 . .
C5 C6 N7 106.0(5) . .
C5 C6 H6 127.0 . .
N7 C6 H6 127.0 . .
Cl19 C17 Cl18 110.0(13) . .
Cl19 C17 H17A 109.7 . .
Cl18 C17 H17A 109.7 . .
Cl19 C17 H17B 109.7 . .
Cl18 C17 H17B 109.7 . .
H17A C17 H17B 108.2 . .
Cl21 C20 Cl22 107(3) . .
Cl21 C20 H20A 110.2 . .
Cl22 C20 H20A 110.2 . .
Cl21 C20 H20B 110.2 . .
Cl22 C20 H20B 110.2 . .
H20A C20 H20B 108.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N4 2.238(5) 6
Cd1 N4 2.238(5) .
Cd1 I2 2.7350(8) .
Cd1 I3 2.7364(8) .
C14 C15 1.391(8) .
C14 C13 1.396(8) .
C14 C14 1.498(10) 2_557
C10 N7 1.472(7) .
C10 C11 1.523(7) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C8 N4 1.337(7) .
C8 N7 1.345(7) .
C8 C9 1.480(8) .
C16 C15 1.384(8) .
C16 C11 1.389(8) .
C16 H16 0.9500 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C15 H15 0.9500 .
N7 C6 1.368(7) .
N4 C5 1.365(8) .
C11 C12 1.381(8) .
C12 C13 1.384(8) .
C12 H12 0.9500 .
C5 C6 1.341(9) .
C5 H5 0.9500 .
C13 H13 0.9500 .
Cl18 C17 1.799(19) .
C6 H6 0.9500 .
Cl21 C20 1.78(2) .
C17 Cl19 1.789(19) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C20 Cl22 1.78(2) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
