#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:17:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180421 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/90/7209007.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_7209007
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, 2(C H4 O)'
_chemical_formula_sum            'C46 H52 Br4 Cd2 N8 O2'
_chemical_formula_weight         1293.40
_chemical_name_common            2_2MeOH
_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                 114.179(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.179(2)
_cell_length_b                   15.8014(19)
_cell_length_c                   9.6965(11)
_cell_measurement_reflns_used    3447
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.192
_cell_measurement_theta_min      2.303
_cell_volume                     2401.2(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 0.990
_diffrn_measured_fraction_theta_max 0.977
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7519
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    4.260
_exptl_absorpt_correction_T_max  0.464
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.874
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0487P)²+4.5953P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                2549
_reflns_number_total             2861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26404h.txt
_cod_data_source_block           2
_cod_original_cell_volume        2401.3(5)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7209007
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 0.27359(2) 0.0000 0.57848(3) 0.01818(10) Uani 1 2 d S
Br2 Br 0.11043(3) 0.0000 0.47312(5) 0.02213(12) Uani 1 2 d S
Br3 Br 0.35956(4) 0.0000 0.86713(5) 0.03580(16) Uani 1 2 d S
N4 N 0.31796(16) 0.11886(16) 0.5130(3) 0.0186(5) Uani 1 1 d .
C5 C 0.3862(2) 0.1665(2) 0.6077(4) 0.0231(7) Uani 1 1 d .
H5 H 0.4237 0.1514 0.7078 0.028 Uiso 1 1 calc R
C6 C 0.3912(2) 0.2377(2) 0.5358(4) 0.0249(7) Uani 1 1 d .
H6 H 0.4321 0.2817 0.5748 0.030 Uiso 1 1 calc R
N7 N 0.32478(16) 0.23426(16) 0.3938(3) 0.0184(5) Uani 1 1 d .
C8 C 0.28195(19) 0.16110(19) 0.3839(3) 0.0170(6) Uani 1 1 d .
C9 C 0.2062(2) 0.1336(2) 0.2495(4) 0.0257(7) Uani 1 1 d .
H9A H 0.1875 0.0780 0.2689 0.039 Uiso 1 1 calc R
H9B H 0.2209 0.1299 0.1621 0.039 Uiso 1 1 calc R
H9C H 0.1600 0.1747 0.2285 0.039 Uiso 1 1 calc R
C10 C 0.3061(2) 0.2994(2) 0.2768(4) 0.0219(7) Uani 1 1 d .
H10A H 0.3108 0.3559 0.3238 0.026 Uiso 1 1 calc R
H10B H 0.2467 0.2925 0.2012 0.026 Uiso 1 1 calc R
C11 C 0.36571(19) 0.29555(18) 0.1974(3) 0.0181(6) Uani 1 1 d .
C12 C 0.4124(2) 0.36672(19) 0.1944(3) 0.0200(6) Uani 1 1 d .
H12 H 0.4081 0.4168 0.2449 0.024 Uiso 1 1 calc R
C13 C 0.46534(19) 0.36515(18) 0.1181(3) 0.0182(6) Uani 1 1 d .
H13 H 0.4969 0.4143 0.1171 0.022 Uiso 1 1 calc R
C14 C 0.47275(18) 0.29266(18) 0.0432(3) 0.0159(6) Uani 1 1 d .
C15 C 0.42762(19) 0.22034(19) 0.0500(3) 0.0179(6) Uani 1 1 d .
H15 H 0.4334 0.1697 0.0022 0.021 Uiso 1 1 calc R
C16 C 0.3745(2) 0.22173(19) 0.1259(3) 0.0189(6) Uani 1 1 d .
H16 H 0.3439 0.1722 0.1293 0.023 Uiso 1 1 calc R
C17 C 0.4235(4) 0.0000 0.2989(7) 0.0454(14) Uani 1 2 d S
H17A H 0.4404 0.0577 0.3364 0.068 Uiso 0.50 1 calc PR
H17B H 0.4601 -0.0205 0.2506 0.068 Uiso 0.50 1 calc PR
H17C H 0.4296 -0.0372 0.3836 0.068 Uiso 0.50 1 calc PR
O18 O 0.3372(3) 0.0000 0.1920(5) 0.0477(10) Uani 1 2 d S
H18 H 0.3333 -0.0255 0.1134 0.057 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'
O O 0.0106 0.0060 '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 115.95(13) . 6
N4 Cd1 Br2 109.55(7) . .
N4 Cd1 Br2 109.55(7) 6 .
N4 Cd1 Br3 101.54(7) . .
N4 Cd1 Br3 101.54(7) 6 .
Br2 Cd1 Br3 118.73(2) . .
C8 N4 C5 107.1(3) . .
C8 N4 Cd1 127.9(2) . .
C5 N4 Cd1 124.8(2) . .
C6 C5 N4 109.2(3) . .
C6 C5 H5 125.4 . .
N4 C5 H5 125.4 . .
C5 C6 N7 106.3(3) . .
C5 C6 H6 126.8 . .
N7 C6 H6 126.8 . .
C8 N7 C6 107.9(3) . .
C8 N7 C10 127.2(3) . .
C6 N7 C10 124.9(3) . .
N4 C8 N7 109.4(3) . .
N4 C8 C9 125.8(3) . .
N7 C8 C9 124.7(3) . .
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(2) . .
N7 C10 H10A 109.1 . .
C11 C10 H10A 109.1 . .
N7 C10 H10B 109.1 . .
C11 C10 H10B 109.1 . .
H10A C10 H10B 107.8 . .
C12 C11 C16 119.1(3) . .
C12 C11 C10 119.6(3) . .
C16 C11 C10 121.3(3) . .
C13 C12 C11 120.5(3) . .
C13 C12 H12 119.8 . .
C11 C12 H12 119.8 . .
C12 C13 C14 120.9(3) . .
C12 C13 H13 119.5 . .
C14 C13 H13 119.5 . .
C13 C14 C15 118.5(3) . .
C13 C14 C14 120.46(19) . 2_655
C15 C14 C14 121.00(19) . 2_655
C16 C15 C14 120.7(3) . .
C16 C15 H15 119.7 . .
C14 C15 H15 119.7 . .
C15 C16 C11 120.3(3) . .
C15 C16 H16 119.8 . .
C11 C16 H16 119.8 . .
O18 C17 H17A 109.5 . .
O18 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
O18 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C17 O18 H18 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N4 2.215(3) .
Cd1 N4 2.215(3) 6
Cd1 Br2 2.5602(6) .
Cd1 Br3 2.5747(6) .
N4 C8 1.327(4) .
N4 C5 1.379(4) .
C5 C6 1.346(5) .
C5 H5 0.9500 .
C6 N7 1.383(4) .
C6 H6 0.9500 .
N7 C8 1.352(4) .
N7 C10 1.467(4) .
C8 C9 1.480(4) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.514(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.389(4) .
C11 C16 1.396(4) .
C12 C13 1.387(4) .
C12 H12 0.9500 .
C13 C14 1.390(4) .
C13 H13 0.9500 .
C14 C15 1.398(4) .
C14 C14 1.490(6) 2_655
C15 C16 1.388(4) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 O18 1.419(7) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
O18 H18 0.8400 .
