#------------------------------------------------------------------------------
#$Date: 2016-04-05 18:14:15 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181588 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/43/7224385.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_7224385
loop_
_publ_author_name
'Li, Lei'
'Tong, Jian'
'Guo, Fang'
'Martí-Rujas, Javier'
_publ_section_title
;
 Crystal engineering of a hybrid metal--organic host framework and its
 single-crystal-to-single-crystal guest exchange using second sphere
 coordination
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              2284
_journal_paper_doi               10.1039/C5CE02093J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C54 H68.4 Br10 Cd N9 O0.7'
_chemical_formula_weight         1766.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-18 deposited with the CCDC.
2016-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.31(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5850(19)
_cell_length_b                   24.232(5)
_cell_length_c                   14.047(3)
_cell_measurement_reflns_used    7784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.53
_cell_measurement_theta_min      1.5
_cell_volume                     3253.4(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD Pilatus 6M-Dectris'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_number            4721
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.497
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         1.585
_diffrn_source                   'Alba-CELLS, Barcelona, Catalonia'
_exptl_absorpt_coefficient_mu    8.048
_exptl_absorpt_correction_T_max  0.1346
_exptl_absorpt_correction_T_min  0.1294
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       block
_exptl_crystal_F_000             1718
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.147
_refine_diff_density_min         -2.223
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4721
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1511P)²+9.9189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2281
_refine_ls_wR_factor_ref         0.2343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3986
_reflns_number_total             4721
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce02093j2.cif
_cod_data_source_block           1G2
_cod_depositor_comments
'Adding full bibliography for 7224384--7224385.cif.'
_cod_original_formula_sum        'C54 H68.40 Br10 Cd N9 O0.70'
_cod_database_code               7224385
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.180
_shelx_estimated_absorpt_t_max   0.828
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br1 Br 0.71580(12) 0.7500 0.24114(9) 0.0370(4) Uani 1 2 d S T P
Br2 Br 0.97024(13) 0.7500 0.03961(9) 0.0412(4) Uani 1 2 d S T P
Br3 Br 1.27086(12) 0.7500 0.23670(9) 0.0360(4) Uani 1 2 d S T P
Br4 Br 1.01767(13) 0.7500 0.43790(9) 0.0416(4) Uani 1 2 d S T P
Br5 Br 0.99221(8) 0.62880(4) 0.23855(6) 0.0398(3) Uani 1 1 d . . .
Br6 Br 0.51590(15) 0.7500 0.48579(11) 0.0553(5) Uani 1 2 d S T P
Br7 Br 0.49809(8) 0.59523(4) 0.23982(7) 0.0452(4) Uani 1 1 d . . .
Br8 Br 0.45947(17) 0.7500 0.99216(12) 0.0614(5) Uani 1 2 d S T P
C1 C 0.2630(9) 0.6179(4) 0.4801(7) 0.039(2) Uani 1 1 d . . .
C2 C 0.1358(10) 0.5932(5) 0.4905(8) 0.055(3) Uani 1 1 d . . .
H2 H 0.0603 0.5978 0.4434 0.066 Uiso 1 1 calc R U .
C3 C 0.1205(9) 0.5618(4) 0.5706(7) 0.047(2) Uani 1 1 d . . .
H3 H 0.0332 0.5443 0.5780 0.056 Uiso 1 1 calc R U .
C4 C 0.2293(9) 0.5549(4) 0.6411(6) 0.038(2) Uani 1 1 d . . .
C5 C 0.3549(10) 0.5775(5) 0.6242(7) 0.058(3) Uani 1 1 d . . .
H5 H 0.4329 0.5711 0.6686 0.070 Uiso 1 1 calc R U .
C6 C 0.3728(10) 0.6091(5) 0.5459(7) 0.055(3) Uani 1 1 d . . .
H6 H 0.4616 0.6249 0.5370 0.066 Uiso 1 1 calc R U .
C7 C 0.2096(10) 0.5219(4) 0.7321(6) 0.043(2) Uani 1 1 d . . .
H7A H 0.1170 0.5037 0.7258 0.052 Uiso 1 1 calc R U .
H7B H 0.2817 0.4926 0.7387 0.052 Uiso 1 1 calc R U .
C8 C 0.2195(9) 0.5568(4) 0.8219(6) 0.039(2) Uani 1 1 d . . .
C9 C 0.2633(11) 0.5333(4) 0.9097(8) 0.053(3) Uani 1 1 d . . .
H9 H 0.2881 0.4954 0.9119 0.064 Uiso 1 1 calc R U .
C10 C 0.2719(12) 0.5629(4) 0.9923(8) 0.058(3) Uani 1 1 d . . .
H10 H 0.3042 0.5460 1.0510 0.069 Uiso 1 1 calc R U .
C11 C 0.2328(10) 0.6182(4) 0.9896(7) 0.046(2) Uani 1 1 d . . .
C12 C 0.1908(10) 0.6434(4) 0.9060(7) 0.050(2) Uani 1 1 d . . .
H12 H 0.1655 0.6813 0.9050 0.060 Uiso 1 1 calc R U .
C13 C 0.1852(10) 0.6123(4) 0.8205(7) 0.046(2) Uani 1 1 d . . .
H13 H 0.1577 0.6297 0.7614 0.055 Uiso 1 1 calc R U .
C14 C 0.7515(10) 0.6221(4) 0.4920(7) 0.046(2) Uani 1 1 d . . .
C15 C 0.8011(10) 0.6456(4) 0.5773(7) 0.052(2) Uani 1 1 d . . .
H15 H 0.8301 0.6831 0.5797 0.063 Uiso 1 1 calc R U .
C16 C 0.8079(10) 0.6132(4) 0.6607(7) 0.049(2) Uani 1 1 d . . .
H16 H 0.8427 0.6290 0.7196 0.059 Uiso 1 1 calc R U .
C17 C 0.7642(9) 0.5579(4) 0.6583(7) 0.042(2) Uani 1 1 d . . .
C18 C 0.7143(11) 0.5371(4) 0.5697(7) 0.050(2) Uani 1 1 d . . .
H18 H 0.6842 0.4997 0.5666 0.060 Uiso 1 1 calc R U .
C19 C 0.7059(11) 0.5671(4) 0.4871(7) 0.052(3) Uani 1 1 d . . .
H19 H 0.6705 0.5512 0.4283 0.063 Uiso 1 1 calc R U .
C20 C 0.7756(10) 0.5215(4) 0.7475(7) 0.047(2) Uani 1 1 d . . .
H20A H 0.7050 0.4917 0.7401 0.056 Uiso 1 1 calc R U .
H20B H 0.8693 0.5042 0.7539 0.056 Uiso 1 1 calc R U .
C21 C 0.7533(9) 0.5542(4) 0.8379(6) 0.041(2) Uani 1 1 d . . .
C22 C 0.8620(10) 0.5644(5) 0.9060(9) 0.064(3) Uani 1 1 d . . .
H22 H 0.9511 0.5484 0.8987 0.077 Uiso 1 1 calc R U .
C23 C 0.8438(11) 0.5968(5) 0.9831(8) 0.065(3) Uani 1 1 d . . .
H23 H 0.9206 0.6040 1.0282 0.078 Uiso 1 1 calc R U .
C24 C 0.7172(9) 0.6188(4) 0.9961(7) 0.041(2) Uani 1 1 d . . .
C25 C 0.6085(11) 0.6056(6) 0.9351(8) 0.072(4) Uani 1 1 d . . .
H25 H 0.5182 0.6193 0.9458 0.086 Uiso 1 1 calc R U .
C26 C 0.6249(10) 0.5724(6) 0.8568(8) 0.070(4) Uani 1 1 d . . .
H26 H 0.5455 0.5623 0.8160 0.083 Uiso 1 1 calc R U .
C1S C 0.0547(11) 0.7500 0.7237(10) 0.035(3) Uani 1 2 d DS T P
C3S C 0.187(2) 0.7500 0.6763(16) 0.20(2) Uani 1 2 d DS T P
H3S1 H 0.2619 0.7342 0.7194 0.307 Uiso 0.5 1 calc R U P
H3S2 H 0.2117 0.7880 0.6601 0.307 Uiso 0.5 1 calc R U P
H3S3 H 0.1760 0.7278 0.6179 0.307 Uiso 0.5 1 calc R U P
Cd1 Cd 0.99327(7) 0.7500 0.23812(6) 0.0368(3) Uani 1 2 d S T P
N1 N 0.2458(9) 0.6513(4) 1.0780(6) 0.056(2) Uani 1 1 d . . .
H1A H 0.2835 0.6847 1.0656 0.083 Uiso 1 1 calc R U .
H1B H 0.3022 0.6334 1.1230 0.083 Uiso 1 1 calc R U .
H1C H 0.1597 0.6561 1.0999 0.083 Uiso 1 1 calc R U .
N2 N 0.2815(8) 0.6527(3) 0.3948(5) 0.0437(18) Uani 1 1 d . . .
H2A H 0.3213 0.6323 0.3498 0.066 Uiso 1 1 calc R U .
H2B H 0.3379 0.6819 0.4118 0.066 Uiso 1 1 calc R U .
H2C H 0.1967 0.6654 0.3707 0.066 Uiso 1 1 calc R U .
N3 N 0.6983(8) 0.6547(3) 1.0806(6) 0.053(2) Uani 1 1 d . . .
H3A H 0.6481 0.6852 1.0617 0.080 Uiso 1 1 calc R U .
H3B H 0.7836 0.6652 1.1074 0.080 Uiso 1 1 calc R U .
H3C H 0.6519 0.6356 1.1242 0.080 Uiso 1 1 calc R U .
N4 N 0.7405(9) 0.6560(3) 0.4057(6) 0.051(2) Uani 1 1 d . . .
H4A H 0.7127 0.6347 0.3545 0.077 Uiso 1 1 calc R U .
H4B H 0.8254 0.6713 0.3968 0.077 Uiso 1 1 calc R U .
H4C H 0.6767 0.6833 0.4121 0.077 Uiso 1 1 calc R U .
N1S N -0.0471(14) 0.7500 0.7532(10) 0.118(8) Uani 1 2 d DS T P
O1S O 0.757(2) 0.7500 0.8109(14) 0.112(7) Uani 0.7 2 d S T P
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
C6 C1 C2 120.3(9) . .
C6 C1 N2 120.2(8) . .
C2 C1 N2 119.5(8) . .
C3 C2 C1 118.5(9) . .
C2 C3 C4 121.8(9) . .
C5 C4 C3 116.9(9) . .
C5 C4 C7 121.5(8) . .
C3 C4 C7 121.6(8) . .
C6 C5 C4 122.3(9) . .
C5 C6 C1 119.9(9) . .
C8 C7 C4 113.6(8) . .
C13 C8 C9 117.8(9) . .
C13 C8 C7 122.0(8) . .
C9 C8 C7 120.3(8) . .
C10 C9 C8 122.3(9) . .
C9 C10 C11 118.9(10) . .
C12 C11 C10 121.3(10) . .
C12 C11 N1 119.0(9) . .
C10 C11 N1 119.6(9) . .
C11 C12 C13 119.0(9) . .
C8 C13 C12 120.7(9) . .
C19 C14 C15 121.5(9) . .
C19 C14 N4 119.4(9) . .
C15 C14 N4 119.0(9) . .
C14 C15 C16 118.8(9) . .
C15 C16 C17 121.2(9) . .
C18 C17 C16 116.7(9) . .
C18 C17 C20 121.4(9) . .
C16 C17 C20 121.8(9) . .
C19 C18 C17 124.0(9) . .
C18 C19 C14 117.8(9) . .
C21 C20 C17 112.2(8) . .
C26 C21 C22 117.1(9) . .
C26 C21 C20 121.3(9) . .
C22 C21 C20 121.5(8) . .
C23 C22 C21 121.3(10) . .
C24 C23 C22 120.4(10) . .
C25 C24 C23 118.9(9) . .
C25 C24 N3 120.9(8) . .
C23 C24 N3 120.1(9) . .
C24 C25 C26 121.3(10) . .
C21 C26 C25 120.4(10) . .
N1S C1S C3S 175.5(19) . .
Br3 Cd1 Br1 179.52(5) . .
Br3 Cd1 Br2 89.80(5) . .
Br1 Cd1 Br2 90.68(5) . .
Br3 Cd1 Br4 89.96(5) . .
Br1 Cd1 Br4 89.56(5) . .
Br2 Cd1 Br4 179.76(4) . .
Br3 Cd1 Br5 90.206(19) . 4_575
Br1 Cd1 Br5 89.793(19) . 4_575
Br2 Cd1 Br5 90.12(2) . 4_575
Br4 Cd1 Br5 89.88(2) . 4_575
Br3 Cd1 Br5 90.206(19) . .
Br1 Cd1 Br5 89.793(19) . .
Br2 Cd1 Br5 90.12(2) . .
Br4 Cd1 Br5 89.88(2) . .
Br5 Cd1 Br5 179.53(4) 4_575 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Cd1 2.6631(14) .
Br2 Cd1 2.7806(16) .
Br3 Cd1 2.6623(14) .
Br4 Cd1 2.7984(16) .
Br5 Cd1 2.9369(11) .
C1 C6 1.364(13) .
C1 C2 1.376(14) .
C1 N2 1.487(11) .
C2 C3 1.376(14) .
C3 C4 1.394(13) .
C4 C5 1.360(13) .
C4 C7 1.531(13) .
C5 C6 1.361(14) .
C7 C8 1.516(13) .
C8 C13 1.384(13) .
C8 C9 1.393(14) .
C9 C10 1.362(15) .
C10 C11 1.391(15) .
C11 C12 1.357(14) .
C11 N1 1.476(12) .
C12 C13 1.416(14) .
C14 C19 1.401(14) .
C14 C15 1.379(14) .
C14 N4 1.463(12) .
C15 C16 1.409(14) .
C16 C17 1.403(14) .
C17 C18 1.393(14) .
C17 C20 1.529(13) .
C18 C19 1.367(14) .
C20 C21 1.525(13) .
C21 C26 1.352(13) .
C21 C22 1.382(14) .
C22 C23 1.360(15) .
C23 C24 1.351(14) .
C24 C25 1.337(15) .
C24 N3 1.494(12) .
C25 C26 1.381(15) .
C1S N1S 1.089(10) .
C1S C3S 1.478(10) .
Cd1 Br5 2.9369(11) 4_575
