#------------------------------------------------------------------------------
#$Date: 2025-08-22 14:50:14 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301863 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/90/7209008.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_7209008
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 Br4 Cd2 N8, 0.87(C S2)'
_chemical_formula_sum            'C44.87 H44 Br4 Cd2 N8 S1.74'
_chemical_formula_weight         1295.77
_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                 114.457(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.478(2)
_cell_length_b                   15.809(2)
_cell_length_c                   9.3913(13)
_cell_measurement_reflns_used    2041
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.38
_cell_volume                     2362.1(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      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.976
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7179
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.414
_exptl_absorpt_correction_T_max  0.8432
_exptl_absorpt_correction_T_min  0.4050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1266.2
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.131
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0439
_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)+(0.0470P)²+7.4320P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                2197
_reflns_number_total             2749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26404h.txt
_cod_data_source_block           3
_cod_original_cell_volume        2362.1(6)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7209008
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 0.27107(3) 0.5000 1.09371(5) 0.01555(14) Uani 1 2 d S
Br2 Br 0.10944(4) 0.5000 0.96313(8) 0.01922(17) Uani 1 2 d S
Br3 Br 0.33290(5) 0.5000 1.39231(8) 0.0286(2) Uani 1 2 d S
N4 N 0.3170(2) 0.6157(2) 1.0218(4) 0.0167(8) Uani 1 1 d .
C5 C 0.3823(3) 0.6646(4) 1.1214(6) 0.0264(12) Uani 1 1 d .
H5 H 0.4180 0.6502 1.2263 0.032 Uiso 1 1 calc R
C6 C 0.3879(3) 0.7354(4) 1.0488(6) 0.0263(12) Uani 1 1 d .
H6 H 0.4276 0.7798 1.0913 0.032 Uiso 1 1 calc R
N7 N 0.3247(2) 0.7314(2) 0.8999(4) 0.0154(8) Uani 1 1 d .
C8 C 0.2836(3) 0.6579(3) 0.8879(5) 0.0155(9) Uani 1 1 d .
C9 C 0.2125(3) 0.6279(3) 0.7440(6) 0.0271(12) Uani 1 1 d .
H9A H 0.2344 0.5980 0.6774 0.041 Uiso 1 1 calc R
H9B H 0.1788 0.6764 0.6870 0.041 Uiso 1 1 calc R
H9C H 0.1772 0.5894 0.7727 0.041 Uiso 1 1 calc R
C10 C 0.3077(3) 0.7972(3) 0.7810(6) 0.0194(10) Uani 1 1 d .
H10B H 0.3130 0.8533 0.8308 0.023 Uiso 1 1 calc R
H10A H 0.2491 0.7913 0.7018 0.023 Uiso 1 1 calc R
C11 C 0.3668(3) 0.7929(3) 0.6998(5) 0.0146(9) Uani 1 1 d .
C12 C 0.4122(3) 0.8639(3) 0.6970(5) 0.0152(9) Uani 1 1 d .
H12 H 0.4074 0.9138 0.7490 0.018 Uiso 1 1 calc R
C13 C 0.4645(3) 0.8635(3) 0.6195(5) 0.0146(9) Uani 1 1 d .
H13 H 0.4947 0.9132 0.6180 0.017 Uiso 1 1 calc R
C14 C 0.4731(2) 0.7906(3) 0.5437(5) 0.0118(9) Uani 1 1 d .
C15 C 0.4284(3) 0.7183(3) 0.5499(5) 0.0142(9) Uani 1 1 d .
H15 H 0.4339 0.6677 0.5005 0.017 Uiso 1 1 calc R
C16 C 0.3762(3) 0.7200(3) 0.6275(5) 0.0148(9) Uani 1 1 d .
H16 H 0.3465 0.6703 0.6311 0.018 Uiso 1 1 calc R
C17 C 0.5000 0.5000 1.0000 0.034(3) Uani 0.87 4 d SP
S18 S 0.44664(18) 0.5000 0.8216(3) 0.0474(7) Uani 0.87 2 d SP
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N4 Cd1 N4 111.5(2) . 6_565
N4 Cd1 Br3 107.05(10) . .
N4 Cd1 Br3 107.05(10) 6_565 .
N4 Cd1 Br2 108.66(9) . .
N4 Cd1 Br2 108.66(9) 6_565 .
Br3 Cd1 Br2 113.92(3) . .
C8 N4 C5 106.1(4) . .
C8 N4 Cd1 129.3(3) . .
C5 N4 Cd1 124.1(3) . .
C6 C5 N4 109.9(4) . .
C6 C5 H5 125.1 . .
N4 C5 H5 125.1 . .
C5 C6 N7 106.4(4) . .
C5 C6 H6 126.8 . .
N7 C6 H6 126.8 . .
C8 N7 C6 107.5(4) . .
C8 N7 C10 128.0(4) . .
C6 N7 C10 124.5(4) . .
N4 C8 N7 110.2(4) . .
N4 C8 C9 125.1(4) . .
N7 C8 C9 124.7(4) . .
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 112.7(4) . .
N7 C10 H10B 109.0 . .
C11 C10 H10B 109.0 . .
N7 C10 H10A 109.0 . .
C11 C10 H10A 109.0 . .
H10B C10 H10A 107.8 . .
C12 C11 C16 118.8(4) . .
C12 C11 C10 119.3(4) . .
C16 C11 C10 121.9(4) . .
C11 C12 C13 121.1(4) . .
C11 C12 H12 119.5 . .
C13 C12 H12 119.5 . .
C12 C13 C14 120.4(4) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
C13 C14 C15 118.2(4) . .
C13 C14 C14 120.7(3) . 2_656
C15 C14 C14 121.1(3) . 2_656
C16 C15 C14 120.5(4) . .
C16 C15 H15 119.8 . .
C14 C15 H15 119.8 . .
C11 C16 C15 120.9(4) . .
C11 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
S18 C17 S18 179.997(1) 5_667 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N4 2.212(4) .
Cd1 N4 2.212(4) 6_565
Cd1 Br3 2.5539(9) .
Cd1 Br2 2.5722(8) .
N4 C8 1.327(6) .
N4 C5 1.376(6) .
C5 C6 1.335(7) .
C5 H5 0.9500 .
C6 N7 1.378(6) .
C6 H6 0.9500 .
N7 C8 1.346(6) .
N7 C10 1.464(6) .
C8 C9 1.486(6) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.518(6) .
C10 H10B 0.9900 .
C10 H10A 0.9900 .
C11 C12 1.381(6) .
C11 C16 1.383(6) .
C12 C13 1.384(6) .
C12 H12 0.9500 .
C13 C14 1.395(6) .
C13 H13 0.9500 .
C14 C15 1.400(6) .
C14 C14 1.483(8) 2_656
C15 C16 1.382(6) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 S18 1.544(3) 5_667
C17 S18 1.544(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N4 Cd1 N4 C8 87.4(4) 6_565 .
Br3 Cd1 N4 C8 -155.8(4) . .
Br2 Cd1 N4 C8 -32.4(4) . .
N4 Cd1 N4 C5 -102.2(4) 6_565 .
Br3 Cd1 N4 C5 14.6(4) . .
Br2 Cd1 N4 C5 138.0(4) . .
C8 N4 C5 C6 0.3(6) . .
Cd1 N4 C5 C6 -172.0(3) . .
N4 C5 C6 N7 0.1(6) . .
C5 C6 N7 C8 -0.4(5) . .
C5 C6 N7 C10 179.3(4) . .
C5 N4 C8 N7 -0.5(5) . .
Cd1 N4 C8 N7 171.2(3) . .
C5 N4 C8 C9 178.1(5) . .
Cd1 N4 C8 C9 -10.1(7) . .
C6 N7 C8 N4 0.6(5) . .
C10 N7 C8 N4 -179.1(4) . .
C6 N7 C8 C9 -178.1(5) . .
C10 N7 C8 C9 2.2(7) . .
C8 N7 C10 C11 -100.5(5) . .
C6 N7 C10 C11 79.9(6) . .
N7 C10 C11 C12 -125.4(4) . .
N7 C10 C11 C16 55.0(6) . .
C16 C11 C12 C13 1.8(6) . .
C10 C11 C12 C13 -177.7(4) . .
C11 C12 C13 C14 -0.7(6) . .
C12 C13 C14 C15 -0.7(6) . .
C12 C13 C14 C14 178.0(4) . 2_656
C13 C14 C15 C16 0.9(6) . .
C14 C14 C15 C16 -177.8(4) 2_656 .
C12 C11 C16 C15 -1.6(6) . .
C10 C11 C16 C15 177.9(4) . .
C14 C15 C16 C11 0.3(6) . .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139196693
