#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:53:12 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179082 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/44/4304411.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_4304411
loop_
_publ_author_name
'Mircea Dincǎ'
'Anne Dailly'
'Charlene Tsay'
'Jeffrey R. Long'
_publ_section_title
;
Expanded Sodalite-Type Metal-Organic Frameworks: Increased Stability
and H2 Adsorption through Ligand-Directed Catenation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11
_journal_page_last               13
_journal_paper_doi               10.1021/ic701917w
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C792 H1096 Cl28 Cu38 N312 O128'
_chemical_formula_sum            'C792 H1096 Cl28 Cu38 N312 O128'
_chemical_formula_weight         20442.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           221
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P 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            1
_cell_length_a                   29.030(4)
_cell_length_b                   29.030(4)
_cell_length_c                   29.030(4)
_cell_measurement_reflns_used    3066
_cell_measurement_temperature    161(2)
_cell_measurement_theta_max      34.162
_cell_measurement_theta_min      4.436
_cell_volume                     24465(6)
_computing_cell_refinement       'Bruker SAINT v7.07b'
_computing_data_collection       'Bruker SMART v5.054d'
_computing_data_reduction        'Bruker SAINT v7.07b'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      161(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       ω/2θ-scans
_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  0.2253
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            86890
_diffrn_reflns_theta_full        20.84
_diffrn_reflns_theta_max         20.84
_diffrn_reflns_theta_min         0.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.8380
_exptl_absorpt_correction_T_min  0.7290
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10634
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   4.777
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      4.777
_refine_ls_R_factor_all          0.1751
_refine_ls_R_factor_gt           0.1254
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3524
_refine_ls_wR_factor_ref         0.3640
_reflns_number_gt                1683
_reflns_number_total             2564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701917w-file002.cif
_cod_data_source_block           md70a
_cod_original_cell_volume        24466(5)
_cod_database_code               4304411
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, -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'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.41256(9) 0.0000 0.5000 0.0423(12) Uani 1 4 d S . .
Cl1 Cl 0.5000 0.0000 0.5000 0.037(3) Uiso 1 16 d S . .
Cl2 Cl 0.3285(3) 0.0000 0.5000 0.098(6) Uani 0.75(2) 4 d SP . .
O1 O 0.5000 0.1311(18) 0.5000 0.175(18) Uiso 0.80 8 d SP . .
O10 O 0.2744(15) 0.1130(15) 0.5000 0.118(17) Uiso 0.40 2 d SP A 1
O2 O 0.2612(17) 0.1001(17) 0.4780(17) 0.054(17) Uiso 0.148(3) 1 d P . 2
Cu2 Cu 0.3348(3) 0.0890(2) 0.5000 0.077(4) Uani 0.296(7) 2 d SP . 2
O3 O 0.3508(18) 0.1598(18) 0.5000 0.15(2) Uiso 0.296(7) 2 d SP . .
O4 O 0.4350(18) 0.2146(12) 0.2146(12) 0.109(18) Uiso 0.25 2 d SP . .
O5 O 0.360(2) 0.0000 0.332(2) 0.17(3) Uiso 0.25 2 d SP . .
O6 O 0.5000 0.1803(17) 0.5000 0.148(15) Uiso 0.80 8 d SP . .
O7 O 0.352(2) 0.248(2) 0.5000 0.13(2) Uiso 0.25 2 d SP . .
O8 O 0.451(2) 0.207(2) 0.5000 0.17(3) Uiso 0.25 2 d SP . .
O9 O 0.534(6) 0.534(6) 0.534(6) 0.25(15) Uiso 0.12 6 d SP . .
O11 O 0.3882(16) 0.353(2) 0.6118(16) 0.20(4) Uiso 0.25 2 d SP . .
N1 N 0.4172(3) 0.0475(3) 0.5505(3) 0.039(3) Uani 1 1 d . . .
N2 N 0.3884(3) 0.0828(3) 0.5569(3) 0.049(3) Uani 1 1 d . . .
C1 C 0.4053(4) 0.1032(5) 0.5947(4) 0.053(5) Uani 1 2 d S . .
C2 C 0.3844(5) 0.1450(6) 0.6156(5) 0.065(5) Uani 1 2 d S . .
C3 C 0.3648(12) 0.1781(11) 0.5866(10) 0.083(10) Uani 0.50 1 d P . .
C3A C 0.3354(11) 0.1523(10) 0.6096(10) 0.075(9) Uani 0.50 1 d P . .
C4 C 0.3129(13) 0.1883(12) 0.6311(12) 0.098(12) Uani 0.50 1 d P . .
C4A C 0.3416(13) 0.2159(11) 0.6094(12) 0.095(13) Uani 0.50 1 d P . .
C5 C 0.3445(6) 0.2229(6) 0.6555(6) 0.089(7) Uani 1 2 d S . .
C6 C 0.3221(5) 0.2645(7) 0.6779(5) 0.103(8) Uani 1 2 d S . .
C7 C 0.3406(7) 0.2843(5) 0.7157(5) 0.101(8) Uani 1 2 d S . .
H7 H 0.3675 0.2711 0.7289 0.121 Uiso 1 2 calc SR . .
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
_geom_angle_publ_flag
N1 Cu1 N1 86.2(4) 4_556 26_556 ?
N1 Cu1 N1 172.3(5) 4_556 . ?
N1 Cu1 N1 93.2(4) 26_556 . ?
N1 Cu1 N1 93.2(4) 4_556 27 ?
N1 Cu1 N1 172.3(5) 26_556 27 ?
N1 Cu1 N1 86.2(4) . 27 ?
N1 Cu1 Cl2 93.9(2) 4_556 . ?
N1 Cu1 Cl2 93.9(2) 26_556 . ?
N1 Cu1 Cl2 93.9(2) . . ?
N1 Cu1 Cl2 93.9(2) 27 . ?
N1 Cu1 Cl1 86.1(2) 4_556 . ?
N1 Cu1 Cl1 86.1(2) 26_556 . ?
N1 Cu1 Cl1 86.1(2) . . ?
N1 Cu1 Cl1 86.1(2) 27 . ?
Cl2 Cu1 Cl1 180.0 . . ?
Cu1 Cl1 Cu1 90.0 45_655 25_656 ?
Cu1 Cl1 Cu1 90.0 45_655 . ?
Cu1 Cl1 Cu1 180.0 25_656 . ?
Cu1 Cl1 Cu1 180.0 45_655 21_556 ?
Cu1 Cl1 Cu1 90.0 25_656 21_556 ?
Cu1 Cl1 Cu1 90.0 . 21_556 ?
Cu1 Cl2 Cu2 85.9(3) . . ?
Cu1 Cl2 Cu2 85.9(3) . 27 ?
Cu2 Cl2 Cu2 171.9(5) . 27 ?
O2 O2 Cu2 73.5(12) 26_556 . ?
O3 Cu2 O2 94.0(19) . . ?
O3 Cu2 O2 94.0(19) . 26_556 ?
O2 Cu2 O2 33(2) . 26_556 ?
O3 Cu2 N2 85.7(11) . 26_556 ?
O2 Cu2 N2 117.0(13) . 26_556 ?
O2 Cu2 N2 149.9(13) 26_556 26_556 ?
O3 Cu2 N2 85.7(11) . . ?
O2 Cu2 N2 149.9(13) . . ?
O2 Cu2 N2 117.0(13) 26_556 . ?
N2 Cu2 N2 93.1(5) 26_556 . ?
O3 Cu2 Cl2 171.3(15) . . ?
O2 Cu2 Cl2 94.3(13) . . ?
O2 Cu2 Cl2 94.3(13) 26_556 . ?
N2 Cu2 Cl2 88.3(3) 26_556 . ?
N2 Cu2 Cl2 88.3(3) . . ?
O1 O6 O8 119(3) . 3_656 ?
O1 O6 O8 119(3) . 23_655 ?
O8 O6 O8 77(2) 3_656 23_655 ?
O1 O6 O8 119(3) . . ?
O8 O6 O8 123(6) 3_656 . ?
O8 O6 O8 77(2) 23_655 . ?
O1 O6 O8 119(3) . 21_556 ?
O8 O6 O8 77(2) 3_656 21_556 ?
O8 O6 O8 123(6) 23_655 21_556 ?
O8 O6 O8 77(2) . 21_556 ?
O11 O11 O11 60.000(14) 8_656 11_566 ?
N1 N1 N2 110.1(5) 46_656 . ?
N1 N1 Cu1 124.2(2) 46_656 . ?
N2 N1 Cu1 125.7(6) . . ?
N1 N2 C1 103.0(10) . . ?
N1 N2 Cu2 112.7(6) . . ?
C1 N2 Cu2 144.1(9) . . ?
N2 C1 N2 113.8(15) 46_656 . ?
N2 C1 C2 123.1(7) 46_656 . ?
N2 C1 C2 123.1(7) . . ?
C3 C2 C3 91(3) 46_656 . ?
C3 C2 C3A 122.7(18) 46_656 . ?
C3 C2 C3A 55.1(15) . . ?
C3 C2 C3A 55.1(15) 46_656 46_656 ?
C3 C2 C3A 122.7(18) . 46_656 ?
C3A C2 C3A 102(3) . 46_656 ?
C3 C2 C1 118.7(16) 46_656 . ?
C3 C2 C1 118.7(16) . . ?
C3A C2 C1 118.1(14) . . ?
C3A C2 C1 118.1(14) 46_656 . ?
C3A C3 C2 64(2) . . ?
C3A C3 C4A 84(3) . . ?
C2 C3 C4A 116(3) . . ?
C3A C3 C3 96(2) . 46_656 ?
C2 C3 C3 44.4(16) . 46_656 ?
C4A C3 C3 90.3(16) . 46_656 ?
C3A C3 C4 43.2(18) . . ?
C2 C3 C4 91(2) . . ?
C4A C3 C4 41.0(18) . . ?
C3 C3 C4 94.3(12) 46_656 . ?
C3 C3A C4 96(3) . . ?
C3 C3A C2 61(2) . . ?
C4 C3A C2 121(3) . . ?
C3 C3A C4A 51(2) . . ?
C4 C3A C4A 45.2(19) . . ?
C2 C3A C4A 93(2) . . ?
C4A C4 C3A 87(3) . . ?
C4A C4 C5 56(2) . . ?
C3A C4 C5 115(3) . . ?
C4A C4 C3 46(2) . . ?
C3A C4 C3 40.7(18) . . ?
C5 C4 C3 87(2) . . ?
C4 C4A C5 70(3) . . ?
C4 C4A C3 93(3) . . ?
C5 C4A C3 122(2) . . ?
C4 C4A C3A 48(2) . . ?
C5 C4A C3A 99(3) . . ?
C3 C4A C3A 44.9(16) . . ?
C4 C4A C4A 96(2) . 46_656 ?
C5 C4A C4A 42.1(18) . 46_656 ?
C3 C4A C4A 89.7(16) . 46_656 ?
C3A C4A C4A 93.8(12) . 46_656 ?
C4A C5 C4A 96(4) 46_656 . ?
C4A C5 C6 121.0(15) 46_656 . ?
C4A C5 C6 121.0(15) . . ?
C4A C5 C4 121.5(19) 46_656 . ?
C4A C5 C4 53.9(18) . . ?
C6 C5 C4 117.5(18) . . ?
C4A C5 C4 53.9(18) 46_656 46_656 ?
C4A C5 C4 121.5(19) . 46_656 ?
C6 C5 C4 117.5(18) . 46_656 ?
C4 C5 C4 97(3) . 46_656 ?
C7 C6 C7 117.7(19) . 11_566 ?
C7 C6 C5 121.1(9) . . ?
C7 C6 C5 121.1(9) 11_566 . ?
C6 C7 C6 122.2(19) . 8_656 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.017(8) 4_556 ?
Cu1 N1 2.017(8) 26_556 ?
Cu1 N1 2.017(8) . ?
Cu1 N1 2.017(8) 27 ?
Cu1 Cl2 2.442(9) . ?
Cu1 Cl1 2.538(3) . ?
Cl1 Cu1 2.538(3) 45_655 ?
Cl1 Cu1 2.538(3) 25_656 ?
Cl1 Cu1 2.538(3) 21_556 ?
Cl2 Cu2 2.589(7) . ?
Cl2 Cu2 2.589(7) 27 ?
O1 O6 1.43(5) . ?
O2 O2 1.28(10) 26_556 ?
O2 Cu2 2.25(5) . ?
Cu2 O3 2.11(5) . ?
Cu2 O2 2.25(5) 26_556 ?
Cu2 N2 2.277(11) 26_556 ?
Cu2 N2 2.277(11) . ?
O5 O5 1.13(13) 22 ?
O6 O8 1.63(6) 3_656 ?
O6 O8 1.63(6) 23_655 ?
O6 O8 1.63(6) . ?
O6 O8 1.63(6) 21_556 ?
O11 O11 1.43(11) 8_656 ?
O11 O11 1.43(11) 11_566 ?
N1 N1 1.324(14) 46_656 ?
N1 N2 1.338(10) . ?
N2 C1 1.340(11) . ?
C1 N2 1.340(11) 46_656 ?
C1 C2 1.49(2) . ?
C2 C3 1.40(3) 46_656 ?
C2 C3 1.40(3) . ?
C2 C3A 1.45(3) . ?
C2 C3A 1.45(3) 46_656 ?
C3 C3A 1.32(4) . ?
C3 C4A 1.45(4) . ?
C3 C3 2.00(6) 46_656 ?
C3 C4 2.01(5) . ?
C3A C4 1.38(4) . ?
C3A C4A 1.86(4) . ?
C4 C4A 1.32(4) . ?
C4 C5 1.53(4) . ?
C4A C5 1.36(3) . ?
C4A C4A 2.01(6) 46_656 ?
C5 C4A 1.36(3) 46_656 ?
C5 C6 1.52(2) . ?
C5 C4 1.53(4) 46_656 ?
C6 C7 1.351(10) . ?
C6 C7 1.351(10) 11_566 ?
C7 C6 1.351(10) 8_656 ?
