#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:17:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180421 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/90/7209013.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_7209013
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'
_chemical_formula_sum            'C44 H44 Cd2 I4 N8'
_chemical_formula_weight         1417.27
_chemical_name_common            3_vac
_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                 113.628(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.081(2)
_cell_length_b                   16.3388(18)
_cell_length_c                   9.3220(10)
_cell_measurement_reflns_used    3760
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.46
_cell_volume                     2523.1(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      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7407
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    3.327
_exptl_absorpt_correction_T_max  0.6515
_exptl_absorpt_correction_T_min  0.4754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.145
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0520
_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)+(0.0858P)²+12.6910P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                2348
_reflns_number_total             2674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26404h.txt
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7209013
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
Cd1 Cd 0.23285(4) 0.0000 0.41769(7) 0.0442(2) Uani 1 2 d S
I2 I 0.39689(4) 0.0000 0.55093(8) 0.0614(2) Uani 1 2 d S
I3 I 0.17197(6) 0.0000 0.09756(8) 0.0729(3) Uani 1 2 d S
C14 C 0.0268(3) 0.2880(3) 0.9571(6) 0.0380(11) Uani 1 1 d .
N7 N 0.1732(3) 0.2258(3) 0.6011(6) 0.0495(12) Uani 1 1 d .
C15 C 0.0672(4) 0.2176(4) 0.9467(7) 0.0453(13) Uani 1 1 d .
H15 H 0.0604 0.1696 0.9935 0.054 Uiso 1 1 calc R
C12 C 0.0880(4) 0.3583(4) 0.8039(8) 0.0499(14) Uani 1 1 d .
H12 H 0.0938 0.4059 0.7548 0.060 Uiso 1 1 calc R
N4 N 0.1851(3) 0.1119(4) 0.4889(6) 0.0521(13) Uani 1 1 d .
C13 C 0.0372(4) 0.3579(4) 0.8840(7) 0.0464(13) Uani 1 1 d .
H13 H 0.0099 0.4055 0.8882 0.056 Uiso 1 1 calc R
C8 C 0.2158(4) 0.1563(4) 0.6176(7) 0.0460(13) Uani 1 1 d .
C16 C 0.1180(4) 0.2184(4) 0.8662(8) 0.0503(14) Uani 1 1 d .
H16 H 0.1443 0.1706 0.8594 0.060 Uiso 1 1 calc R
C10 C 0.1858(5) 0.2914(4) 0.7140(10) 0.0615(18) Uani 1 1 d .
H10A H 0.1793 0.3434 0.6602 0.074 Uiso 1 1 calc R
H10B H 0.2410 0.2886 0.7915 0.074 Uiso 1 1 calc R
C11 C 0.1295(4) 0.2890(4) 0.7970(7) 0.0462(13) Uani 1 1 d .
C9 C 0.2853(5) 0.1315(6) 0.7615(10) 0.076(2) Uani 1 1 d .
H9A H 0.2659 0.1056 0.8323 0.115 Uiso 1 1 calc R
H9B H 0.3164 0.1789 0.8107 0.115 Uiso 1 1 calc R
H9C H 0.3185 0.0938 0.7349 0.115 Uiso 1 1 calc R
C5 C 0.1201(5) 0.1556(6) 0.3880(8) 0.074(2) Uani 1 1 d .
H5 H 0.0863 0.1391 0.2874 0.089 Uiso 1 1 calc R
C6 C 0.1125(6) 0.2257(6) 0.4567(9) 0.079(3) Uani 1 1 d .
H6 H 0.0735 0.2659 0.4137 0.095 Uiso 1 1 calc R
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'
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 109.9(3) . 6
N4 Cd1 I2 110.19(14) . .
N4 Cd1 I2 110.20(14) 6 .
N4 Cd1 I3 106.83(14) . .
N4 Cd1 I3 106.83(14) 6 .
I2 Cd1 I3 112.76(3) . .
C13 C14 C15 118.1(5) . .
C13 C14 C14 120.9(4) . 2_557
C15 C14 C14 120.9(4) . 2_557
C8 N7 C6 108.2(6) . .
C8 N7 C10 128.5(6) . .
C6 N7 C10 123.4(6) . .
C14 C15 C16 120.5(5) . .
C14 C15 H15 119.7 . .
C16 C15 H15 119.7 . .
C11 C12 C13 120.6(6) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C8 N4 C5 105.7(6) . .
C8 N4 Cd1 130.4(4) . .
C5 N4 Cd1 123.2(5) . .
C14 C13 C12 121.1(5) . .
C14 C13 H13 119.4 . .
C12 C13 H13 119.4 . .
N4 C8 N7 110.3(6) . .
N4 C8 C9 124.7(6) . .
N7 C8 C9 125.0(6) . .
C11 C16 C15 120.9(5) . .
C11 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
N7 C10 C11 114.2(6) . .
N7 C10 H10A 108.7 . .
C11 C10 H10A 108.7 . .
N7 C10 H10B 108.7 . .
C11 C10 H10B 108.7 . .
H10A C10 H10B 107.6 . .
C12 C11 C16 118.7(5) . .
C12 C11 C10 119.8(6) . .
C16 C11 C10 121.5(6) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C6 C5 N4 109.8(7) . .
C6 C5 H5 125.1 . .
N4 C5 H5 125.1 . .
C5 C6 N7 106.1(6) . .
C5 C6 H6 126.9 . .
N7 C6 H6 126.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N4 2.234(6) .
Cd1 N4 2.234(6) 6
Cd1 I2 2.7179(10) .
Cd1 I3 2.7357(9) .
C14 C13 1.381(8) .
C14 C15 1.386(8) .
C14 C14 1.483(10) 2_557
N7 C8 1.346(8) .
N7 C6 1.354(10) .
N7 C10 1.454(9) .
C15 C16 1.399(8) .
C15 H15 0.9300 .
C12 C11 1.375(9) .
C12 C13 1.396(8) .
C12 H12 0.9300 .
N4 C8 1.319(8) .
N4 C5 1.375(9) .
C13 H13 0.9300 .
C8 C9 1.480(10) .
C16 C11 1.378(9) .
C16 H16 0.9300 .
C10 C11 1.507(8) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C5 C6 1.346(12) .
C5 H5 0.9300 .
C6 H6 0.9300 .
