#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/45/4114576.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_4114576
loop_
_publ_author_name
'Mohamed Eddaoudi'
'Jaheon Kim'
'Michael O'Keeffe'
'Omar M. Yaghi'
_publ_contact_author
;
Omar M. Yaghi
Department of Chemistry
University of Michigan
930 N. University Ave.
Ann Arbor, MI 48109-1055, USA
;
_publ_contact_author_email       oyaghi@umich.edu
_publ_section_title
;
 Cu2[o-Br-C6H3(CO2)2]2(H2O)2.(DMF)8(H2O)2: A Framework Deliberately
 Designed To Have the NbO Structure Type
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              376
_journal_page_last               377
_journal_paper_doi               10.1021/ja017154e
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C40 H70 Br2 Cu2 N8 O20'
_chemical_formula_weight         1269.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           229
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   21.607(3)
_cell_length_b                   21.607(3)
_cell_length_c                   21.607(3)
_cell_measurement_reflns_used    1244
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      15.25
_cell_measurement_theta_min      2.31
_cell_volume                     10087(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       'omega & phi 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  0.3281
_diffrn_reflns_av_sigmaI/netI    0.0889
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33854
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.884
_exptl_absorpt_correction_T_max  0.9423
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             3924
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         752
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1693
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          1.349
_refine_ls_shift/su_mean         0.115
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1699P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2215
_refine_ls_wR_factor_ref         0.2840
_reflns_number_gt                321
_reflns_number_total             752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017154e_s2.cif
_cod_data_source_block           MOF-101
_cod_original_cell_volume        10088(2)
_cod_original_formula_sum        'C40 H70 N8 O20 Cu2 Br2'
_cod_database_code               4114576
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu Cu 0.0000 0.0000 0.43841(14) 0.0756(14) Uani 1 8 d S
O1 O 0.0899(4) 0.0000 0.4480(4) 0.091(3) Uani 1 2 d S
O2 O 0.0000 0.0000 0.3396(8) 0.137(7) Uani 1 8 d S
C1 C 0.1147(8) 0.0000 0.5000 0.084(6) Uani 1 4 d S
C2 C 0.1844(8) 0.0000 0.5000 0.092(5) Uani 1 4 d S
C3 C 0.2145(14) 0.0000 0.4466(14) 0.127(13) Uani 0.50 2 d SP
C4 C 0.2162(14) 0.0511(14) 0.5000 0.150(18) Uani 0.50 2 d SP
Br Br 0.1770(4) 0.1309(4) 0.5000 0.387(12) Uani 0.25 2 d SP
O3 O 0.0000 0.188(5) 0.274(5) 0.48(6) Uiso 0.25 2 d SP
O4 O 0.051(3) 0.051(3) 0.051(3) 0.28(7) Uiso 0.25 6 d SP
O1S O 0.0331(18) 0.0331(18) 0.235(4) 0.37(3) Uiso 0.25 2 d SPD
N1S N 0.111(4) 0.111(4) 0.292(5) 0.37(3) Uiso 0.25 2 d SPD
C1S C 0.073(2) 0.073(2) 0.248(6) 0.37(3) Uiso 0.25 2 d SPD
C2S C 0.105(3) 0.170(3) 0.326(5) 0.37(3) Uiso 0.25 1 d PD
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'
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
O1 Cu O1 167.9(5) 62 61
O1 Cu O1 89.36(5) 62 2
O1 Cu O1 89.36(6) 61 2
O1 Cu O1 89.36(6) 62 .
O1 Cu O1 89.36(5) 61 .
O1 Cu O1 167.9(5) 2 .
O1 Cu O2 96.1(3) 62 .
O1 Cu O2 96.1(3) 61 .
O1 Cu O2 96.1(3) 2 .
O1 Cu O2 96.1(3) . .
O1 Cu Cu 83.9(3) 62 49_556
O1 Cu Cu 83.9(3) 61 49_556
O1 Cu Cu 83.9(3) 2 49_556
O1 Cu Cu 83.9(3) . 49_556
O2 Cu Cu 180.000(1) . 49_556
C1 O1 Cu 121.6(10) . .
O1 C1 O1 129.0(18) . 50_556
O1 C1 C2 115.5(9) . .
O1 C1 C2 115.5(9) 50_556 .
C4 C2 C4 116(3) 51 .
C4 C2 C3 75.0(10) 51 50_556
C4 C2 C3 75.0(10) . 50_556
C4 C2 C3 75.0(10) 51 .
C4 C2 C3 75.0(10) . .
C3 C2 C3 121(3) 50_556 .
C4 C2 C1 121.9(15) 51 .
C4 C2 C1 121.9(15) . .
C3 C2 C1 119.4(15) 50_556 .
C3 C2 C1 119.4(15) . .
C2 C3 C4 118(3) . 43
C2 C3 C4 51.8(17) . 51
C4 C3 C4 87(2) 43 51
C2 C3 C4 51.8(17) . .
C4 C3 C4 87(2) 43 .
C4 C3 C4 87(3) 51 .
C2 C4 C3 124(3) . 89
C2 C4 C3 53.2(16) . 50_556
C3 C4 C3 93(2) 89 50_556
C2 C4 C3 53.2(16) . .
C3 C4 C3 93(2) 89 .
C3 C4 C3 92(3) 50_556 .
C2 C4 Br 122(2) . .
C3 C4 Br 114(3) 89 .
C3 C4 Br 127.6(15) 50_556 .
C3 C4 Br 127.6(15) . .
Br Br C4 161.2(10) 13_556 .
C1S O1S O1S 133.5(19) . 52
C1S O1S O1S 133.6(19) . 51
O1S O1S O1S 89.997(3) 52 51
C1S N1S C2S 137.8(18) . .
C1S N1S C2S 136.7(17) . 62
C2S N1S C2S 85(3) . 62
O1S C1S N1S 154(10) . .
N1S C2S C2S 47.7(17) . 62
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O1 1.954(8) 62
Cu O1 1.954(8) 61
Cu O1 1.954(8) 2
Cu O1 1.954(8) .
Cu O2 2.135(18) .
Cu Cu 2.662(6) 49_556
O1 C1 1.245(9) .
C1 O1 1.245(9) 50_556
C1 C2 1.51(2) .
C2 C4 1.30(3) 51
C2 C4 1.30(3) .
C2 C3 1.32(3) 50_556
C2 C3 1.32(3) .
C3 C4 1.50(3) 43
C3 C4 1.60(2) 51
C3 C4 1.60(2) .
C4 C3 1.50(3) 89
C4 C3 1.60(2) 50_556
C4 Br 1.92(3) .
Br Br 1.410(17) 13_556
O1S C1S 1.262(11) .
O1S O1S 1.43(8) 52
O1S O1S 1.45(8) 51
N1S C1S 1.486(11) .
N1S C2S 1.466(11) .
N1S C2S 1.483(11) 62
C2S C2S 2.00(7) 62
