#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:10:05 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179442 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/39/4333934.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_4333934
loop_
_publ_author_name
'Christopher R. Murdock'
'Zheng Lu'
'David M. Jenkins'
_publ_section_title
;
 Effects of Solvation on the Framework of a Breathing Copper MOF Employing
 a Semirigid Linker
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2182
_journal_page_last               2187
_journal_paper_doi               10.1021/ic3026304
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C16 H20 Br2 Cu2 N12 O4 S'
_chemical_formula_weight         763.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.55(3)
_cell_angle_beta                 76.47(3)
_cell_angle_gamma                76.55(3)
_cell_formula_units_Z            1
_cell_length_a                   7.260(16)
_cell_length_b                   11.77(3)
_cell_length_c                   13.15(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1035(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX II'
_diffrn_measurement_method       'ω scan'
_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  0.1421
_diffrn_reflns_av_sigmaI/netI    0.2760
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7844
_diffrn_reflns_theta_full        23.34
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    3.036
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       needle
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         2.499
_refine_diff_density_min         -1.760
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2839
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.2125
_refine_ls_R_factor_gt           0.1711
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.1554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3766
_refine_ls_wR_factor_ref         0.4152
_reflns_number_gt                1470
_reflns_number_total             2839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3026304_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        1036(4)
_cod_database_code               4333934
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
O9 O 0.624(7) 0.873(3) 0.887(5) 0.28(3) Uani 0.50 1 d PD
O9A O 0.772(7) 0.628(6) 1.017(3) 0.28(3) Uani 0.50 1 d PD
O9B O 0.918(5) 0.693(5) 0.774(3) 0.28(3) Uani 0.50 1 d PD
O9C O 0.507(6) 0.651(5) 0.860(4) 0.28(3) Uani 0.50 1 d PD
Br1 Br 0.3413(4) -0.1299(2) 0.3993(2) 0.0569(10) Uani 1 1 d .
S3 S 0.703(2) 0.712(3) 0.8839(12) 0.137(10) Uani 0.50 1 d PD
C1 C 0.041(3) 0.2516(15) 0.4124(14) 0.025(2) Uani 1 1 d .
H1 H -0.0900 0.2736 0.4033 0.030 Uiso 1 1 calc R
C2 C 0.339(3) 0.2543(15) 0.4109(14) 0.025(2) Uani 1 1 d .
H2 H 0.4606 0.2773 0.3999 0.030 Uiso 1 1 calc R
C3 C 0.130(3) 0.4621(17) 0.3488(17) 0.047(3) Uani 1 1 d .
H3A H 0.0443 0.4836 0.2954 0.056 Uiso 1 1 calc R
H3B H 0.2524 0.4902 0.3132 0.056 Uiso 1 1 calc R
C4 C 0.024(3) 0.5293(19) 0.4528(16) 0.047(3) Uani 1 1 d .
H4 H -0.0014 0.6143 0.4391 0.056 Uiso 1 1 calc R
C5 C 0.036(3) -0.0746(15) 0.7379(15) 0.025(2) Uani 1 1 d .
H5 H -0.0951 -0.0836 0.7622 0.030 Uiso 1 1 calc R
C6 C 0.327(3) -0.0718(15) 0.7372(15) 0.025(2) Uani 1 1 d .
H6 H 0.4431 -0.0775 0.7608 0.030 Uiso 1 1 calc R
C7 C 0.125(3) -0.1230(18) 0.9192(17) 0.047(3) Uani 1 1 d .
H7A H 0.2409 -0.1767 0.9430 0.056 Uiso 1 1 calc R
H7B H 0.0163 -0.1676 0.9458 0.056 Uiso 1 1 calc R
C8 C 0.077(3) -0.0118(18) 0.9680(17) 0.047(3) Uani 1 1 d .
H8 H 0.1679 0.0405 0.9493 0.056 Uiso 1 1 calc R
N1 N 0.310(2) 0.1500(15) 0.4469(11) 0.029(4) Uani 1 1 d .
N2 N 0.117(2) 0.1491(15) 0.4458(11) 0.032(4) Uani 1 1 d .
N3 N 0.1663(19) 0.3349(12) 0.3883(11) 0.021(2) Uani 1 1 d .
N4 N 0.307(2) -0.0438(12) 0.6325(11) 0.019(3) Uani 1 1 d .
N5 N 0.118(2) -0.0438(11) 0.6313(11) 0.021(4) Uani 1 1 d .
N6 N 0.1577(19) -0.0904(12) 0.8030(11) 0.021(2) Uani 1 1 d .
Cu2 Cu 0.0000 0.0000 0.5000 0.0206(9) Uani 1 2 d S
Cu3 Cu 0.5000 0.0000 0.5000 0.0215(10) Uani 1 2 d S
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'
Cu Cu 0.3201 1.2651 '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'
S S 0.1246 0.1234 '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
Cu2 Br1 Cu3 79.70(17) . .
O9C S3 O9 110.8(13) . .
O9C S3 O9B 109.1(13) . .
O9 S3 O9B 109.6(13) . .
O9C S3 O9A 109.7(12) . .
O9 S3 O9A 108.4(13) . .
O9B S3 O9A 109.3(13) . .
N2 C1 N3 113.1(16) . .
N2 C1 H1 123.4 . .
N3 C1 H1 123.4 . .
N1 C2 N3 110.9(16) . .
N1 C2 H2 124.5 . .
N3 C2 H2 124.5 . .
N3 C3 C4 109.4(16) . .
N3 C3 H3A 109.8 . .
C4 C3 H3A 109.8 . .
N3 C3 H3B 109.8 . .
C4 C3 H3B 109.8 . .
H3A C3 H3B 108.3 . .
C4 C4 C3 123(3) 2_566 .
C4 C4 H4 118.7 2_566 .
C3 C4 H4 118.7 . .
N6 C5 N5 112.9(16) . .
N6 C5 H5 123.5 . .
N5 C5 H5 123.5 . .
N6 C6 N4 110.7(16) . .
N6 C6 H6 124.6 . .
N4 C6 H6 124.6 . .
N6 C7 C8 111.7(16) . .
N6 C7 H7A 109.3 . .
C8 C7 H7A 109.3 . .
N6 C7 H7B 109.3 . .
C8 C7 H7B 109.3 . .
H7A C7 H7B 107.9 . .
C8 C8 C7 122(3) 2_557 .
C8 C8 H8 119.0 2_557 .
C7 C8 H8 119.0 . .
C2 N1 N2 108.5(15) . .
C2 N1 Cu3 128.0(12) . .
N2 N1 Cu3 123.5(12) . .
C1 N2 N1 107.8(16) . .
C1 N2 Cu2 129.1(13) . .
N1 N2 Cu2 123.1(12) . .
C1 N3 C2 99.5(14) . .
C1 N3 C3 129.6(16) . .
C2 N3 C3 130.8(16) . .
C6 N4 N5 107.2(13) . .
C6 N4 Cu3 129.3(12) . .
N5 N4 Cu3 123.4(10) . .
N4 N5 C5 104.3(13) . .
N4 N5 Cu2 125.4(10) . .
C5 N5 Cu2 130.3(12) . .
C5 N6 C6 104.8(15) . .
C5 N6 C7 129.0(16) . .
C6 N6 C7 126.3(16) . .
N5 Cu2 N5 180.000(1) . 2_556
N5 Cu2 N2 90.8(6) . .
N5 Cu2 N2 89.2(6) 2_556 .
N5 Cu2 N2 89.2(6) . 2_556
N5 Cu2 N2 90.8(6) 2_556 2_556
N2 Cu2 N2 180.0(9) . 2_556
N5 Cu2 Br1 92.4(5) . 2_556
N5 Cu2 Br1 87.6(5) 2_556 2_556
N2 Cu2 Br1 90.7(5) . 2_556
N2 Cu2 Br1 89.3(5) 2_556 2_556
N5 Cu2 Br1 87.6(5) . .
N5 Cu2 Br1 92.4(5) 2_556 .
N2 Cu2 Br1 89.3(5) . .
N2 Cu2 Br1 90.7(5) 2_556 .
Br1 Cu2 Br1 180.0 2_556 .
N4 Cu3 N4 180.000(1) 2_656 .
N4 Cu3 N1 89.8(5) 2_656 .
N4 Cu3 N1 90.2(5) . .
N4 Cu3 N1 90.2(5) 2_656 2_656
N4 Cu3 N1 89.8(5) . 2_656
N1 Cu3 N1 180.0(8) . 2_656
N4 Cu3 Br1 91.7(4) 2_656 .
N4 Cu3 Br1 88.3(4) . .
N1 Cu3 Br1 88.9(5) . .
N1 Cu3 Br1 91.1(5) 2_656 .
N4 Cu3 Br1 88.3(4) 2_656 2_656
N4 Cu3 Br1 91.7(4) . 2_656
N1 Cu3 Br1 91.1(5) . 2_656
N1 Cu3 Br1 88.9(5) 2_656 2_656
Br1 Cu3 Br1 180.0 . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O9 S3 1.862(19) .
O9A S3 1.877(18) .
O9B S3 1.875(18) .
O9C S3 1.860(18) .
Br1 Cu2 2.831(5) .
Br1 Cu3 2.834(5) .
C1 N2 1.21(2) .
C1 N3 1.42(2) .
C1 H1 0.9500 .
C2 N1 1.24(2) .
C2 N3 1.43(2) .
C2 H2 0.9500 .
C3 N3 1.43(2) .
C3 C4 1.70(3) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C4 1.26(4) 2_566
C4 H4 0.9500 .
C5 N6 1.32(2) .
C5 N5 1.38(2) .
C5 H5 0.9500 .
C6 N6 1.35(2) .
C6 N4 1.36(2) .
C6 H6 0.9500 .
C7 N6 1.45(3) .
C7 C8 1.54(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C8 1.26(4) 2_557
C8 H8 0.9500 .
N1 N2 1.40(2) .
N1 Cu3 2.043(16) .
N2 Cu2 2.013(17) .
N4 N5 1.37(2) .
N4 Cu3 1.996(14) .
N5 Cu2 1.998(13) .
Cu2 N5 1.998(13) 2_556
Cu2 N2 2.013(17) 2_556
Cu2 Br1 2.831(5) 2_556
Cu3 N4 1.996(14) 2_656
Cu3 N1 2.043(16) 2_656
Cu3 Br1 2.834(5) 2_656
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.079 0.500 0.500 367 180 ' '
