#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:53:12 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179082 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/44/4304413.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_4304413
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         'C456 H360 Cl6 Mn27 N264 O24'
_chemical_formula_sum            'C456 H360 Cl6 Mn27 N264 O24'
_chemical_formula_weight         11618.16
_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            1
_cell_length_a                   29.1071(12)
_cell_length_b                   29.1071(12)
_cell_length_c                   29.1071(12)
_cell_measurement_reflns_used    6044
_cell_measurement_temperature    159(2)
_cell_measurement_theta_max      41.342
_cell_measurement_theta_min      4.425
_cell_volume                     24660.2(18)
_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      159(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  0.1195
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            63047
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_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    0.393
_exptl_absorpt_correction_T_max  0.9115
_exptl_absorpt_correction_T_min  0.9115
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5913
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0625
_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)+(0.0923P)²+51.8828P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1973
_reflns_number_gt                1339
_reflns_number_total             2048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701917w-file004.cif
_cod_data_source_block           md78a
_cod_database_code               4304413
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.0000 0.09438(4) 0.0509(4) Uani 1 4 d S . .
Mn2 Mn 0.4035(12) 0.0000 0.1575(12) 0.181(12) Uiso 0.06 2 d SP . 2
Cl2 Cl 0.5000 0.0000 0.0000 0.0492(8) Uiso 1 16 d S . .
O1 O 0.5000 0.0000 0.1675(3) 0.113(2) Uiso 1 4 d S . .
N1 N 0.44886(9) 0.05617(10) 0.08856(10) 0.0575(8) Uani 1 1 d . . .
N2 N 0.41874(10) 0.06691(10) 0.12099(11) 0.0636(9) Uani 1 1 d . . .
N3 N 0.23662(14) 0.17929(17) 0.23662(14) 0.0813(16) Uani 1 2 d S . .
N4 N 0.4542(6) 0.0344(6) 0.2292(6) 0.105(5) Uiso 0.25 1 d P . 1
C1 C 0.40045(17) 0.10668(14) 0.10668(14) 0.0620(14) Uani 1 2 d S . .
C2 C 0.36479(19) 0.13172(15) 0.13172(15) 0.0682(15) Uani 1 2 d S . .
C3 C 0.34727(15) 0.11493(16) 0.17230(15) 0.0877(15) Uani 1 1 d . . .
H3 H 0.3596 0.0875 0.1850 0.105 Uiso 1 1 calc R . .
C4 C 0.31236(16) 0.13718(17) 0.19465(16) 0.0954(17) Uani 1 1 d . . .
H4 H 0.3007 0.1250 0.2226 0.115 Uiso 1 1 calc R . .
C5 C 0.2940(2) 0.17705(17) 0.17705(17) 0.0784(19) Uani 1 2 d S . .
C6 C 0.2539(2) 0.19899(16) 0.19899(16) 0.0776(19) Uani 1 2 d S . .
C7 C 0.4592(6) 0.0000 0.1920(6) 0.115(5) Uiso 0.50 2 d SP . 1
C8 C 0.4791(5) 0.0792(5) 0.2399(6) 0.170(6) Uiso 0.50 1 d P . 1
N5 N 0.380(2) 0.0000 0.0000 0.15(2) Uiso 0.25 8 d SP . .
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'
Mn Mn 0.3368 0.7283 '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
O1 Mn1 N1 94.38(8) . 52_655 ?
O1 Mn1 N1 94.38(8) . 2_655 ?
N1 Mn1 N1 95.00(15) 52_655 2_655 ?
O1 Mn1 N1 94.38(8) . 51 ?
N1 Mn1 N1 171.24(16) 52_655 51 ?
N1 Mn1 N1 84.33(15) 2_655 51 ?
O1 Mn1 N1 94.38(8) . . ?
N1 Mn1 N1 84.33(15) 52_655 . ?
N1 Mn1 N1 171.24(16) 2_655 . ?
N1 Mn1 N1 95.00(15) 51 . ?
O1 Mn1 Cl2 180.0 . . ?
N1 Mn1 Cl2 85.62(8) 52_655 . ?
N1 Mn1 Cl2 85.62(8) 2_655 . ?
N1 Mn1 Cl2 85.62(8) 51 . ?
N1 Mn1 Cl2 85.62(8) . . ?
N2 Mn2 N2 118.8(16) 51 . ?
Mn1 Cl2 Mn1 90.0 65_655 . ?
Mn1 Cl2 Mn1 90.0 65_655 49_655 ?
Mn1 Cl2 Mn1 180.0 . 49_655 ?
Mn1 Cl2 Mn1 180.0 65_655 17 ?
Mn1 Cl2 Mn1 90.0 . 17 ?
Mn1 Cl2 Mn1 90.0 49_655 17 ?
C7 O1 C7 118.2(16) 2_655 . ?
C7 O1 Mn1 120.9(8) 2_655 . ?
C7 O1 Mn1 120.9(8) . . ?
N2 N1 N1 109.68(17) . 67 ?
N2 N1 Mn1 124.3(2) . . ?
N1 N1 Mn1 125.12(7) 67 . ?
N1 N2 C1 104.2(3) . . ?
N1 N2 Mn2 105.1(8) . . ?
C1 N2 Mn2 144.2(9) . . ?
C6 N3 C6 115.7(5) . 9 ?
N4 N4 C8 69.4(15) 38 38 ?
N4 N4 C7 146.0(10) 38 . ?
C8 N4 C7 110.6(16) 38 . ?
N4 N4 C8 57.9(13) 38 . ?
C8 N4 C8 116.5(15) 38 . ?
C7 N4 C8 132.9(16) . . ?
N2 C1 N2 112.3(4) 67 . ?
N2 C1 C2 123.9(2) 67 . ?
N2 C1 C2 123.9(2) . . ?
C3 C2 C3 118.2(5) . 67 ?
C3 C2 C1 120.9(2) . . ?
C3 C2 C1 120.9(2) 67 . ?
C4 C3 C2 121.0(4) . . ?
C3 C4 C5 120.7(4) . . ?
C4 C5 C4 118.4(5) 67 . ?
C4 C5 C6 120.8(2) 67 . ?
C4 C5 C6 120.8(2) . . ?
N3 C6 N3 124.3(5) . 5 ?
N3 C6 C5 117.9(3) . . ?
N3 C6 C5 117.9(3) 5 . ?
O1 C7 N4 117.4(12) . . ?
O1 C7 N4 117.4(12) . 51 ?
N4 C7 N4 85.0(17) . 51 ?
C8 C8 N4 106.6(10) 52_655 38 ?
C8 C8 N4 118.5(9) 52_655 . ?
N4 C8 N4 52.8(14) 38 . ?
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
Mn1 O1 2.129(8) . ?
Mn1 N1 2.218(3) 52_655 ?
Mn1 N1 2.218(3) 2_655 ?
Mn1 N1 2.218(3) 51 ?
Mn1 N1 2.218(3) . ?
Mn1 Cl2 2.7472(11) . ?
Mn2 N2 2.263(18) 51 ?
Mn2 N2 2.263(18) . ?
Cl2 Mn1 2.7472(11) 65_655 ?
Cl2 Mn1 2.7472(11) 49_655 ?
Cl2 Mn1 2.7472(11) 17 ?
O1 C7 1.385(17) 2_655 ?
O1 C7 1.385(17) . ?
N1 N2 1.325(4) . ?
N1 N1 1.333(6) 67 ?
N2 C1 1.340(4) . ?
N3 C6 1.335(3) . ?
N3 C6 1.335(3) 9 ?
N4 N4 1.30(3) 38 ?
N4 C8 1.38(2) 38 ?
N4 C7 1.48(2) . ?
N4 C8 1.53(2) . ?
C1 N2 1.340(4) 67 ?
C1 C2 1.463(7) . ?
C2 C3 1.376(5) . ?
C2 C3 1.376(5) 67 ?
C3 C4 1.369(5) . ?
C4 C5 1.377(5) . ?
C5 C4 1.377(5) 67 ?
C5 C6 1.475(7) . ?
C6 N3 1.335(3) 5 ?
C7 N4 1.48(2) 51 ?
C8 C8 1.21(3) 52_655 ?
C8 N4 1.38(2) 38 ?
