#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:17:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178893 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/22/4112283.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_4112283
loop_
_publ_author_name
'Brendan F. Abrahams'
'Adrian Hawley'
'Marissa G. Haywood'
'Timothy A. Hudson'
'Richard Robson'
'Damian A. Slizys'
_publ_section_title
;
 Serendipity and Design in the Generation of New Coordination Polymers: An
 Extensive Series of Highly Symmetrical Guanidinium-Templated,
 Carbonate-Based Networks with the Sodalite Topology
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2894
_journal_page_last               2904
_journal_paper_doi               10.1021/ja038904i
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety
;
 (Ca 2+)6, (C O3 2-)12 (K 1+)3, (N C4 H12 1+), (C N3 H6 1+)8, (H2 O)3
;
_chemical_formula_sum            'C24 H66 Ca6 K3 N25 O39'
_chemical_formula_weight         1686.80
_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            2
_cell_length_a                   14.8173(14)
_cell_length_b                   14.8173(14)
_cell_length_c                   14.8173(14)
_cell_measurement_reflns_used    2828
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.75
_cell_volume                     3253.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0122
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8563
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Sheldrick, G. M. SADABS
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       cube
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         321
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0544
_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)+(0.0880P)²+17.9940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                314
_reflns_number_total             321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038904isi20031009_123034.cif
_cod_data_source_block           ca1086ra
_cod_database_code               4112283
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
N3 N 0.0000 0.0000 0.0000 0.076(10) Uani 1 48 d S
O3 O 0.0000 0.0000 0.361(3) 0.19(2) Uiso 0.50 8 d SP
C3 C 0.0000 0.114(11) 0.0000 0.08(4) Uiso 0.17 8 d SP
C4 C 0.0000 0.093(5) 0.037(6) 0.10(4) Uiso 0.13 2 d SP
Ca1 Ca 0.2500 0.0000 0.5000 0.0339(8) Uani 1 8 d S
O1 O 0.0000 -0.2356(3) 0.3422(2) 0.0372(11) Uani 1 2 d S
C1 C 0.0000 -0.3190(3) 0.3190(3) 0.0345(17) Uani 1 4 d S
O2 O 0.1197(2) 0.1197(2) 0.5000 0.0441(15) Uani 1 4 d S
K1 K 0.0000 0.0000 0.4375(6) 0.073(2) Uani 0.50 8 d SP
C2 C 0.1802(4) -0.1802(4) 0.1802(4) 0.045(2) Uani 1 6 d S
N1 N 0.1425(3) -0.1425(3) 0.2520(4) 0.0510(14) Uani 1 2 d SD
H1 H 0.0923(16) -0.162(2) 0.274(3) 0.037(12) Uiso 1 1 d D
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
C4 N3 C4 180(7) 66 18
C4 N3 C4 134(7) 66 .
C4 N3 C4 46(7) 18 .
C4 N3 C4 30(5) 66 53
C4 N3 C4 150(5) 18 53
C4 N3 C4 110(3) . 53
C4 N3 C4 150(5) 66 5
C4 N3 C4 30(5) 18 5
C4 N3 C4 70(3) . 5
C4 N3 C4 180(7) 53 5
C4 N3 C4 70(3) 66 69
C4 N3 C4 110(3) 18 69
C4 N3 C4 150(5) . 69
C4 N3 C4 82(2) 53 69
C4 N3 C4 98(2) 5 69
C4 N3 C4 110(3) 66 21
C4 N3 C4 70(3) 18 21
C4 N3 C4 30(5) . 21
C4 N3 C4 98(2) 53 21
C4 N3 C4 82(2) 5 21
C4 N3 C4 180(7) 69 21
C4 N3 C4 110(3) 66 62
C4 N3 C4 70(3) 18 62
C4 N3 C4 82(2) . 62
C4 N3 C4 134(7) 53 62
C4 N3 C4 46(7) 5 62
C4 N3 C4 110(3) 69 62
C4 N3 C4 70(3) 21 62
C4 N3 C4 46(7) 66 49
C4 N3 C4 134(7) 18 49
C4 N3 C4 180(7) . 49
C4 N3 C4 70(3) 53 49
C4 N3 C4 110(3) 5 49
C4 N3 C4 30(5) 69 49
C4 N3 C4 150(5) 21 49
C4 N3 C4 98(2) 62 49
C4 N3 C4 70(3) 66 14
C4 N3 C4 110(3) 18 14
C4 N3 C4 98(2) . 14
C4 N3 C4 46(7) 53 14
C4 N3 C4 134(7) 5 14
C4 N3 C4 70(3) 69 14
C4 N3 C4 110(3) 21 14
C4 N3 C4 180(7) 62 14
C4 N3 C4 82(2) 49 14
C4 N3 C4 82(2) 66 57
C4 N3 C4 98(2) 18 57
C4 N3 C4 110(3) . 57
C4 N3 C4 70(3) 53 57
C4 N3 C4 110(3) 5 57
C4 N3 C4 46(7) 69 57
C4 N3 C4 134(7) 21 57
C4 N3 C4 150(5) 62 57
C4 N3 C4 70(3) 49 57
C4 N3 C4 30(5) 14 57
C4 N3 C4 98(2) 66 9
C4 N3 C4 82(2) 18 9
C4 N3 C4 70(3) . 9
C4 N3 C4 110(3) 53 9
C4 N3 C4 70(3) 5 9
C4 N3 C4 134(7) 69 9
C4 N3 C4 46(7) 21 9
C4 N3 C4 30(5) 62 9
C4 N3 C4 110(3) 49 9
C4 N3 C4 150(5) 14 9
C4 N3 C4 180(7) 57 9
O1 Ca1 O1 90.473(17) 61 82
O1 Ca1 O1 169.57(18) 61 14_556
O1 Ca1 O1 90.473(17) 82 14_556
O1 Ca1 O1 90.473(17) 61 33_545
O1 Ca1 O1 169.57(18) 82 33_545
O1 Ca1 O1 90.473(17) 14_556 33_545
O1 Ca1 O2 137.80(14) 61 83_545
O1 Ca1 O2 86.16(7) 82 83_545
O1 Ca1 O2 52.63(15) 14_556 83_545
O1 Ca1 O2 86.16(7) 33_545 83_545
O1 Ca1 O2 86.16(7) 61 51
O1 Ca1 O2 137.80(14) 82 51
O1 Ca1 O2 86.16(7) 14_556 51
O1 Ca1 O2 52.63(15) 33_545 51
O2 Ca1 O2 122.83(14) 83_545 51
O1 Ca1 O2 86.16(7) 61 .
O1 Ca1 O2 52.63(15) 82 .
O1 Ca1 O2 86.16(7) 14_556 .
O1 Ca1 O2 137.80(14) 33_545 .
O2 Ca1 O2 122.83(14) 83_545 .
O2 Ca1 O2 85.2(2) 51 .
O1 Ca1 O2 52.63(15) 61 81
O1 Ca1 O2 86.16(7) 82 81
O1 Ca1 O2 137.80(14) 14_556 81
O1 Ca1 O2 86.16(7) 33_545 81
O2 Ca1 O2 85.2(2) 83_545 81
O2 Ca1 O2 122.83(14) 51 81
O2 Ca1 O2 122.83(14) . 81
C1 O1 Ca1 100.3(4) . 29_445
O1 C1 O1 121.0(7) . 66
O1 C1 O2 119.5(3) . 79_445
O1 C1 O2 119.5(3) 66 79_445
C1 O2 Ca1 87.58(11) 82 .
C1 O2 Ca1 87.58(11) 82 77
Ca1 O2 Ca1 175.2(2) . 77
C1 O2 K1 159.7(2) 82 .
Ca1 O2 K1 92.27(11) . .
Ca1 O2 K1 92.27(11) 77 .
C1 O2 K1 159.7(2) 82 49_556
Ca1 O2 K1 92.27(11) . 49_556
Ca1 O2 K1 92.27(11) 77 49_556
K1 O2 K1 40.5(4) . 49_556
O3 K1 O2 110.3(2) . .
O3 K1 O2 110.3(2) . 51
O2 K1 O2 83.11(13) . 51
O3 K1 O2 110.3(2) . 3_556
O2 K1 O2 83.11(13) . 3_556
O2 K1 O2 139.5(4) 51 3_556
O3 K1 O2 110.3(2) . 49_556
O2 K1 O2 139.5(4) . 49_556
O2 K1 O2 83.11(13) 51 49_556
O2 K1 O2 83.11(13) 3_556 49_556
O3 K1 O3 180.000(3) . 49_556
O2 K1 O3 69.7(2) . 49_556
O2 K1 O3 69.7(2) 51 49_556
O2 K1 O3 69.7(2) 3_556 49_556
O2 K1 O3 69.7(2) 49_556 49_556
N1 C2 N1 119.95(4) 6 12
N1 C2 N1 119.95(4) 6 .
N1 C2 N1 119.95(4) 12 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N3 C4 1.48(7) 66
N3 C4 1.48(7) 18
N3 C4 1.48(7) .
N3 C4 1.48(7) 53
N3 C4 1.48(7) 5
N3 C4 1.48(7) 69
N3 C4 1.48(7) 21
N3 C4 1.48(7) 62
N3 C4 1.48(7) 49
N3 C4 1.48(7) 14
N3 C4 1.48(7) 57
N3 C4 1.48(7) 9
O3 K1 2.99(5) 49_556
Ca1 O1 2.348(4) 61
Ca1 O1 2.348(4) 82
Ca1 O1 2.348(4) 14_556
Ca1 O1 2.348(4) 33_545
Ca1 O2 2.6217(3) 83_545
Ca1 O2 2.6217(3) 51
Ca1 O2 2.6217(3) .
Ca1 O2 2.6217(3) 81
O1 C1 1.283(5) .
O1 Ca1 2.348(4) 29_445
C1 O1 1.283(5) 66
C1 O2 1.284(9) 79_445
O2 C1 1.284(9) 82
O2 Ca1 2.6217(3) 77
O2 K1 2.674(6) .
O2 K1 2.674(6) 49_556
K1 O2 2.674(6) 51
K1 O2 2.674(6) 3_556
K1 O2 2.674(6) 49_556
K1 O3 2.99(5) 49_556
C2 N1 1.325(5) 6
C2 N1 1.325(5) 12
C2 N1 1.325(5) .
