#------------------------------------------------------------------------------
#$Date: 2017-09-22 04:33:29 +0300 (Fri, 22 Sep 2017) $
#$Revision: 201152 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/06/7120683.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_7120683
loop_
_publ_author_name
'Nikolayenko, Varvara I.'
'Heyns, Anneli'
'Barbour, Len'
_publ_section_title
;
 Threading the needle: guest transport in a versatile 0D porous molecular
 crystal
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06676G
_journal_year                    2017
_chemical_formula_moiety
'	C35.09 H43.26 Cl4 Cu2 N8 O1.09, 0.912(C H3 O)'
_chemical_formula_sum            'C36 H46 Cl4 Cu2 N8 O2'
_chemical_formula_weight         891.69
_chemical_name_common            1
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-08-18 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.441(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4261(10)
_cell_length_b                   10.7068(13)
_cell_length_c                   21.974(3)
_cell_measurement_reflns_used    4118
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.12
_cell_volume                     1955.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type  'Bruker APEX CCD area -detector'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8066
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.081
_diffrn_reflns_theta_min         2.122
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  0.9331
_exptl_absorpt_correction_T_min  0.8385
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, 2016'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       Plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1216P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1862
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2999
_reflns_number_total             4121
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc06676g2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1955.5(4)
_cod_database_code               7120683
_shelx_shelxl_version_number     2016/6
_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   0.838
_shelx_estimated_absorpt_t_max   0.933
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.02110(6) 0.77241(5) 0.40002(2) 0.0210(2) Uani 1 1 d . . . . .
Cl1 Cl 0.15039(13) 0.80449(10) 0.31831(4) 0.0230(3) Uani 1 1 d . . . . .
Cl2 Cl -0.12415(14) 0.64463(11) 0.45434(5) 0.0324(3) Uani 1 1 d . . . . .
N1 N 0.2225(5) 0.7259(3) 0.45498(14) 0.0187(8) Uani 1 1 d . . . . .
C8 C 0.7617(6) 0.7417(4) 0.70212(17) 0.0188(9) Uani 1 1 d . . . . .
H8 H 0.874912 0.743735 0.715174 0.023 Uiso 1 1 calc R U . . .
C9 C 0.6665(5) 0.8239(4) 0.72963(16) 0.0178(9) Uani 1 1 d . . . . .
C12 C 0.4319(5) 0.7331(4) 0.66586(17) 0.0170(9) Uani 1 1 d . . . . .
C5 C 0.5317(5) 0.6551(4) 0.63778(15) 0.0181(9) Uani 1 1 d . . . . .
N2 N 0.3962(4) 0.6435(3) 0.52985(13) 0.0175(7) Uani 1 1 d . . . . .
N4 N 0.1739(4) 1.1408(3) 0.64050(14) 0.0188(8) Uani 1 1 d . . . . .
C11 C 0.4997(5) 0.8181(4) 0.71149(15) 0.0174(9) Uani 1 1 d . . . . .
C2 C 0.4803(6) 0.7243(4) 0.49942(19) 0.0278(11) Uani 1 1 d . . . . .
H2 H 0.592176 0.742046 0.508498 0.033 Uiso 1 1 calc R U . . .
C6 C 0.6996(5) 0.6576(4) 0.65683(16) 0.0174(8) Uani 1 1 d . . . . .
N3 N 0.3329(4) 1.0078(3) 0.69635(14) 0.0191(8) Uani 1 1 d . . . . .
C10 C 0.7491(6) 0.9157(4) 0.77635(17) 0.0261(10) Uani 1 1 d . . . . .
H10A H 0.864459 0.897133 0.785078 0.039 Uiso 1 1 calc R U . . .
H10B H 0.703489 0.909019 0.814488 0.039 Uiso 1 1 calc R U . . .
H10C H 0.732956 1.000636 0.759888 0.039 Uiso 1 1 calc R U . . .
C4 C 0.4611(5) 0.5707(4) 0.58507(16) 0.0206(9) Uani 1 1 d . . . . .
H4A H 0.545367 0.513291 0.575221 0.025 Uiso 1 1 calc R U . . .
H4B H 0.374055 0.519665 0.597696 0.025 Uiso 1 1 calc R U . . .
C3 C 0.2408(5) 0.6468(4) 0.50156(16) 0.0174(8) Uani 1 1 d . . . . .
H3 H 0.156475 0.598600 0.513639 0.021 Uiso 1 1 calc R U . . .
C1 C 0.3720(6) 0.7741(4) 0.45364(19) 0.0277(11) Uani 1 1 d . . . . .
H1 H 0.396391 0.834104 0.424680 0.033 Uiso 1 1 calc R U . . .
C7 C 0.8121(6) 0.5718(4) 0.63024(18) 0.0231(9) Uani 1 1 d . . . . .
H7A H 0.923234 0.589813 0.649226 0.035 Uiso 1 1 calc R U . . .
H7B H 0.800000 0.584811 0.585572 0.035 Uiso 1 1 calc R U . . .
H7C H 0.786254 0.484857 0.638606 0.035 Uiso 1 1 calc R U . . .
C13 C 0.2510(6) 0.7287(4) 0.64732(18) 0.0228(9) Uani 1 1 d . . . . .
H13A H 0.216797 0.793356 0.616406 0.034 Uiso 1 1 calc R U . . .
H13B H 0.199968 0.743281 0.683672 0.034 Uiso 1 1 calc R U . . .
H13C H 0.219163 0.646424 0.629887 0.034 Uiso 1 1 calc R U . . .
C14 C 0.3926(6) 0.9067(4) 0.73983(16) 0.0215(9) Uani 1 1 d . . . . .
H14A H 0.300239 0.860122 0.751122 0.026 Uiso 1 1 calc R U . . .
H14B H 0.453928 0.943306 0.777963 0.026 Uiso 1 1 calc R U . . .
C17 C 0.1822(5) 1.0473(4) 0.68003(16) 0.0194(9) Uani 1 1 d . . . . .
H17 H 0.092171 1.012674 0.694938 0.023 Uiso 1 1 calc R U . . .
C15 C 0.4300(6) 1.0818(4) 0.66676(18) 0.0247(10) Uani 1 1 d . . . . .
H15 H 0.543619 1.077065 0.669976 0.030 Uiso 1 1 calc R U . . .
C16 C 0.3297(6) 1.1626(4) 0.63212(18) 0.0267(10) Uani 1 1 d . . . . .
H16 H 0.362128 1.224959 0.605960 0.032 Uiso 1 1 calc R U . . .
O1A O -0.0488(9) 1.0278(6) 0.5449(3) 0.042(2) Uani 0.544(10) 1 d D . P A 1
C1A C -0.165(2) 0.9353(18) 0.5474(9) 0.060(6) Uani 0.544(10) 1 d D . P A 1
H1A1 H -0.130382 0.857224 0.530385 0.089 Uiso 0.544(10) 1 calc R U P A 1
H1A2 H -0.267708 0.961949 0.523104 0.089 Uiso 0.544(10) 1 calc R U P A 1
H1A3 H -0.178955 0.922063 0.590325 0.089 Uiso 0.544(10) 1 calc R U P A 1
O1B O 0.0500(11) 1.1260(8) 0.4419(3) 0.036(2) Uani 0.456(10) 1 d . . P A 2
C1B C 0.202(2) 1.0690(15) 0.4354(8) 0.034(4) Uani 0.456(10) 1 d . . P A 2
H1B1 H 0.270208 1.130515 0.418773 0.052 Uiso 0.456(10) 1 calc R U P A 2
H1B2 H 0.183323 0.997740 0.407106 0.052 Uiso 0.456(10) 1 calc R U P A 2
H1B3 H 0.256955 1.040235 0.475765 0.052 Uiso 0.456(10) 1 calc R U P A 2
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 Cu1 N1 164.50(14) 3_576 .
N4 Cu1 Cl1 92.52(9) 3_576 .
N1 Cu1 Cl1 92.63(10) . .
N4 Cu1 Cl2 92.28(10) 3_576 .
N1 Cu1 Cl2 90.55(10) . .
Cl1 Cu1 Cl2 149.96(5) . .
C3 N1 C1 105.6(4) . .
C3 N1 Cu1 127.9(3) . .
C1 N1 Cu1 126.4(3) . .
C6 C8 C9 123.2(4) . .
C6 C8 H8 118.4 . .
C9 C8 H8 118.4 . .
C8 C9 C11 118.1(4) . .
C8 C9 C10 118.2(4) . .
C11 C9 C10 123.6(4) . .
C5 C12 C11 119.9(4) . .
C5 C12 C13 121.0(4) . .
C11 C12 C13 119.1(4) . .
C12 C5 C6 120.3(4) . .
C12 C5 C4 120.3(4) . .
C6 C5 C4 119.3(4) . .
C3 N2 C2 107.5(3) . .
C3 N2 C4 126.4(3) . .
C2 N2 C4 126.1(4) . .
C17 N4 C16 105.5(4) . .
C17 N4 Cu1 127.3(3) . 3_576
C16 N4 Cu1 127.2(3) . 3_576
C9 C11 C12 120.3(4) . .
C9 C11 C14 119.6(4) . .
C12 C11 C14 120.1(4) . .
C1 C2 N2 105.9(4) . .
C1 C2 H2 127.1 . .
N2 C2 H2 127.1 . .
C8 C6 C5 118.1(4) . .
C8 C6 C7 119.3(4) . .
C5 C6 C7 122.6(4) . .
C17 N3 C15 107.7(3) . .
C17 N3 C14 128.1(4) . .
C15 N3 C14 124.2(4) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N2 C4 C5 111.2(3) . .
N2 C4 H4A 109.4 . .
C5 C4 H4A 109.4 . .
N2 C4 H4B 109.4 . .
C5 C4 H4B 109.4 . .
H4A C4 H4B 108.0 . .
N1 C3 N2 110.7(4) . .
N1 C3 H3 124.7 . .
N2 C3 H3 124.7 . .
C2 C1 N1 110.3(4) . .
C2 C1 H1 124.9 . .
N1 C1 H1 124.9 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N3 C14 C11 110.9(3) . .
N3 C14 H14A 109.5 . .
C11 C14 H14A 109.5 . .
N3 C14 H14B 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 108.0 . .
N4 C17 N3 111.4(4) . .
N4 C17 H17 124.3 . .
N3 C17 H17 124.3 . .
C16 C15 N3 105.6(4) . .
C16 C15 H15 127.2 . .
N3 C15 H15 127.2 . .
C15 C16 N4 109.8(4) . .
C15 C16 H16 125.1 . .
N4 C16 H16 125.1 . .
O1A C1A H1A1 109.5 . .
O1A C1A H1A2 109.5 . .
H1A1 C1A H1A2 109.5 . .
O1A C1A H1A3 109.5 . .
H1A1 C1A H1A3 109.5 . .
H1A2 C1A H1A3 109.5 . .
O1B C1B H1B1 109.5 . .
O1B C1B H1B2 109.5 . .
H1B1 C1B H1B2 109.5 . .
O1B C1B H1B3 109.5 . .
H1B1 C1B H1B3 109.5 . .
H1B2 C1B H1B3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N4 1.968(4) 3_576
Cu1 N1 1.979(4) .
Cu1 Cl1 2.2739(10) .
Cu1 Cl2 2.2964(11) .
N1 C3 1.318(5) .
N1 C1 1.366(6) .
C8 C6 1.381(6) .
C8 C9 1.393(6) .
C8 H8 0.9500 .
C9 C11 1.399(6) .
C9 C10 1.507(5) .
C12 C5 1.399(6) .
C12 C11 1.404(6) .
C12 C13 1.512(6) .
C5 C6 1.408(6) .
C5 C4 1.512(5) .
N2 C3 1.355(5) .
N2 C2 1.361(6) .
N2 C4 1.470(5) .
N4 C17 1.320(5) .
N4 C16 1.376(6) .
C11 C14 1.512(5) .
C2 C1 1.352(7) .
C2 H2 0.9500 .
C6 C7 1.505(6) .
N3 C17 1.330(5) .
N3 C15 1.376(5) .
N3 C14 1.476(5) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C3 H3 0.9500 .
C1 H1 0.9500 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C17 H17 0.9500 .
C15 C16 1.353(6) .
C15 H15 0.9500 .
C16 H16 0.9500 .
O1A C1A 1.401(9) .
C1A H1A1 0.9800 .
C1A H1A2 0.9800 .
C1A H1A3 0.9800 .
O1B C1B 1.45(2) .
C1B H1B1 0.9800 .
C1B H1B2 0.9800 .
C1B H1B3 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4B Cl2 0.99 2.84 3.650(5) 139.9 3_566
C3 H3 Cl2 0.95 2.55 3.080(4) 115.1 .
C3 H3 Cl2 0.95 2.72 3.457(4) 134.6 3_566
C14 H14A Cl1 0.99 2.74 3.662(4) 155.7 4_576
C15 H15 Cl1 0.95 2.85 3.703(5) 150.5 3_676
C16 H16 Cl2 0.95 2.62 3.129(5) 114.1 3_576
C1A H1A1 Cl2 0.98 2.83 3.771(17) 161.3 .
C1B H1B2 Cl1 0.98 2.83 3.802(17) 174.0 .
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
C6 C8 C9 C11 1.8(6) .
C6 C8 C9 C10 -177.1(3) .
C11 C12 C5 C6 2.6(5) .
C13 C12 C5 C6 -178.0(3) .
C11 C12 C5 C4 -175.1(3) .
C13 C12 C5 C4 4.3(5) .
C8 C9 C11 C12 -1.3(5) .
C10 C9 C11 C12 177.5(3) .
C8 C9 C11 C14 -179.3(3) .
C10 C9 C11 C14 -0.5(5) .
C5 C12 C11 C9 -0.8(5) .
C13 C12 C11 C9 179.8(3) .
C5 C12 C11 C14 177.2(3) .
C13 C12 C11 C14 -2.2(5) .
C3 N2 C2 C1 0.2(5) .
C4 N2 C2 C1 -177.2(4) .
C9 C8 C6 C5 -0.1(6) .
C9 C8 C6 C7 -179.5(3) .
C12 C5 C6 C8 -2.2(5) .
C4 C5 C6 C8 175.5(3) .
C12 C5 C6 C7 177.3(4) .
C4 C5 C6 C7 -5.1(5) .
C3 N2 C4 C5 -117.9(4) .
C2 N2 C4 C5 59.0(5) .
C12 C5 C4 N2 67.7(5) .
C6 C5 C4 N2 -110.0(4) .
C1 N1 C3 N2 0.2(4) .
Cu1 N1 C3 N2 -177.4(2) .
C2 N2 C3 N1 -0.2(4) .
C4 N2 C3 N1 177.1(3) .
N2 C2 C1 N1 -0.1(5) .
C3 N1 C1 C2 -0.1(5) .
Cu1 N1 C1 C2 177.5(3) .
C17 N3 C14 C11 130.3(4) .
C15 N3 C14 C11 -52.1(5) .
C9 C11 C14 N3 103.9(4) .
C12 C11 C14 N3 -74.1(5) .
C16 N4 C17 N3 -0.9(4) .
Cu1 N4 C17 N3 177.4(2) 3_576
C15 N3 C17 N4 1.4(5) .
C14 N3 C17 N4 179.3(3) .
C17 N3 C15 C16 -1.3(5) .
C14 N3 C15 C16 -179.3(3) .
N3 C15 C16 N4 0.8(5) .
C17 N4 C16 C15 0.0(5) .
Cu1 N4 C16 C15 -178.3(3) 3_576
