#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:17:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180421 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/90/7209011.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_7209011
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 H Cl3'
_chemical_formula_sum            'C45 H45 Cd2 Cl3 I4 N8'
_chemical_formula_weight         1536.64
_chemical_name_common            3_CHCl3
_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                 113.271(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.281(3)
_cell_length_b                   16.193(3)
_cell_length_c                   9.2445(17)
_cell_measurement_reflns_used    2658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.40
_cell_volume                     2514.0(8)
_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 0.989
_diffrn_measured_fraction_theta_max 0.988
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7287
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.502
_exptl_absorpt_correction_T_max  0.7320
_exptl_absorpt_correction_T_min  0.4997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.141
_refine_diff_density_min         -1.626
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2645
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0535
_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)+(0.0687P)²+62.9123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1447
_reflns_number_gt                2353
_reflns_number_total             2645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26404h.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7209011
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 0.73730(5) 0.0000 0.41842(9) 0.0181(2) Uani 1 2 d S
I2 I 0.90007(4) 0.0000 0.55646(8) 0.0222(2) Uani 1 2 d S
I3 I 0.67922(5) 0.0000 0.09621(8) 0.0261(2) Uani 1 2 d S
N4 N 0.6923(4) 0.1162(4) 0.4857(8) 0.0218(14) Uani 1 1 d .
C5 C 0.6352(5) 0.1664(6) 0.3784(10) 0.0302(19) Uani 1 1 d .
H5 H 0.6062 0.1537 0.2704 0.036 Uiso 1 1 calc R
C6 C 0.6271(5) 0.2364(5) 0.4513(10) 0.0278(18) Uani 1 1 d .
H6 H 0.5921 0.2813 0.4055 0.033 Uiso 1 1 calc R
N7 N 0.6797(4) 0.2289(4) 0.6043(7) 0.0191(13) Uani 1 1 d .
C8 C 0.7174(5) 0.1566(5) 0.6209(9) 0.0209(15) Uani 1 1 d .
C9 C 0.7791(5) 0.1249(6) 0.7720(10) 0.031(2) Uani 1 1 d .
H9A H 0.8087 0.1715 0.8362 0.047 Uiso 1 1 calc R
H9B H 0.8158 0.0883 0.7492 0.047 Uiso 1 1 calc R
H9C H 0.7530 0.0942 0.8297 0.047 Uiso 1 1 calc R
C10 C 0.6907(5) 0.2928(5) 0.7233(9) 0.0226(16) Uani 1 1 d .
H10A H 0.6865 0.3476 0.6735 0.027 Uiso 1 1 calc R
H10B H 0.7451 0.2878 0.8063 0.027 Uiso 1 1 calc R
C11 C 0.6311(4) 0.2882(5) 0.7996(8) 0.0185(15) Uani 1 1 d .
C12 C 0.5897(5) 0.3593(5) 0.8088(9) 0.0230(16) Uani 1 1 d .
H12 H 0.5966 0.4089 0.7609 0.028 Uiso 1 1 calc R
C13 C 0.5392(5) 0.3583(5) 0.8864(9) 0.0198(15) Uani 1 1 d .
H13 H 0.5123 0.4076 0.8921 0.024 Uiso 1 1 calc R
C14 C 0.5265(4) 0.2863(5) 0.9573(8) 0.0174(14) Uani 1 1 d .
C15 C 0.5662(5) 0.2141(5) 0.9428(9) 0.0209(15) Uani 1 1 d .
H15 H 0.5574 0.1637 0.9860 0.025 Uiso 1 1 calc R
C16 C 0.6178(5) 0.2156(5) 0.8663(9) 0.0231(16) Uani 1 1 d .
H16 H 0.6445 0.1664 0.8593 0.028 Uiso 1 1 calc R
Cl17 Cl 0.4764(7) 0.0000 0.2798(15) 0.085(3) Uani 0.50 2 d SPDU
Cl18 Cl 0.5123(5) -0.0890(5) 0.5713(9) 0.079(2) Uani 0.50 1 d PDU
C19 C 0.5373(16) 0.0000 0.483(2) 0.056(9) Uani 0.50 2 d SPD
H19 H 0.5951 0.0000 0.5020 0.067 Uiso 0.50 2 calc SPR
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'
O O 0.0106 0.0060 '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 114.5(3) 6 .
N4 Cd1 I2 108.76(17) 6 .
N4 Cd1 I2 108.76(17) . .
N4 Cd1 I3 105.97(17) 6 .
N4 Cd1 I3 105.98(17) . .
I2 Cd1 I3 112.97(4) . .
C8 N4 C5 105.6(7) . .
C8 N4 Cd1 130.6(5) . .
C5 N4 Cd1 123.4(5) . .
C6 C5 N4 109.5(7) . .
C6 C5 H5 125.2 . .
N4 C5 H5 125.2 . .
C5 C6 N7 105.6(7) . .
C5 C6 H6 127.2 . .
N7 C6 H6 127.2 . .
C8 N7 C6 108.5(7) . .
C8 N7 C10 128.4(7) . .
C6 N7 C10 123.1(7) . .
N4 C8 N7 110.8(7) . .
N4 C8 C9 124.4(7) . .
N7 C8 C9 124.8(7) . .
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 . .
N7 C10 C11 113.8(6) . .
N7 C10 H10A 108.8 . .
C11 C10 H10A 108.8 . .
N7 C10 H10B 108.8 . .
C11 C10 H10B 108.8 . .
H10A C10 H10B 107.7 . .
C16 C11 C12 118.3(7) . .
C16 C11 C10 122.1(7) . .
C12 C11 C10 119.6(7) . .
C13 C12 C11 120.9(7) . .
C13 C12 H12 119.6 . .
C11 C12 H12 119.6 . .
C12 C13 C14 121.6(7) . .
C12 C13 H13 119.2 . .
C14 C13 H13 119.2 . .
C13 C14 C15 117.2(7) . .
C13 C14 C14 121.2(5) . 2_657
C15 C14 C14 121.6(5) . 2_657
C16 C15 C14 121.0(7) . .
C16 C15 H15 119.5 . .
C14 C15 H15 119.5 . .
C15 C16 C11 120.9(7) . .
C15 C16 H16 119.5 . .
C11 C16 H16 119.5 . .
Cl18 Cl18 C19 75.4(8) 2_656 2_656
Cl18 Cl18 C19 63.9(7) 2_656 .
C19 Cl18 C19 51.5(17) 2_656 .
Cl18 Cl18 Cl17 131.2(4) 2_656 2_656
C19 Cl18 Cl17 57.9(6) 2_656 2_656
C19 Cl18 Cl17 75.6(8) . 2_656
Cl17 C19 Cl18 108.4(10) . .
Cl17 C19 Cl18 108.4(10) . 6
Cl18 C19 Cl18 106.3(13) . 6
Cl17 C19 H19 111.2 . .
Cl18 C19 H19 111.2 . .
Cl18 C19 H19 111.2 6 .
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(7) 6
Cd1 N4 2.238(7) .
Cd1 I2 2.7354(11) .
Cd1 I3 2.7388(11) .
N4 C8 1.322(10) .
N4 C5 1.384(11) .
C5 C6 1.357(12) .
C5 H5 0.9500 .
C6 N7 1.366(11) .
C6 H6 0.9500 .
N7 C8 1.336(10) .
N7 C10 1.465(10) .
C8 C9 1.497(11) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.516(10) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C16 1.392(11) .
C11 C12 1.398(11) .
C12 C13 1.375(11) .
C12 H12 0.9500 .
C13 C14 1.401(11) .
C13 H13 0.9500 .
C14 C15 1.410(10) .
C14 C14 1.471(15) 2_657
C15 C16 1.384(11) .
C15 H15 0.9500 .
C16 H16 0.9500 .
Cl17 C19 1.768(18) .
Cl18 Cl18 1.214(16) 2_656
Cl18 C19 1.672(15) 2_656
Cl18 C19 1.801(14) .
Cl18 Cl17 1.947(12) 2_656
C19 Cl18 1.801(14) 6
C19 H19 1.0000 .
