#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:07:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179468 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/65/4336593.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_4336593
loop_
_publ_author_name
'Dawei Feng'
'Hai-Long Jiang'
'Ying-Pin Chen'
'Zhi-Yuan Gu'
'Zhangwen Wei'
'Hong-Cai Zhou'
_publ_section_title
;
 Metal-Organic Frameworks Based on Previously Unknown Zr8/Hf8 Cubic
 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12661
_journal_page_last               12667
_journal_paper_doi               10.1021/ic4018536
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C144 H72 Cl0 Co3 Hf8 N12 O30'
_chemical_formula_sum            'C144 H72 Cl0 Co3 Hf8 N12 O30'
_chemical_formula_weight         4054.85
_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                   19.152(3)
_cell_length_b                   19.152(3)
_cell_length_c                   19.152(3)
_cell_measurement_reflns_used    5282
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20.31
_cell_measurement_theta_min      2.38
_cell_volume                     7024.9(19)
_computing_cell_refinement       'SAINT+ ver. (Bruker, 2001)'
_computing_data_collection       'APEX2  (Bruker, 2008)'
_computing_data_reduction        'SAINT+ ver. (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART APEX II 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  0.0938
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65582
_diffrn_reflns_theta_full        24.51
_diffrn_reflns_theta_max         24.51
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    3.151
_exptl_absorpt_correction_T_max  0.3655
_exptl_absorpt_correction_T_min  0.2536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.959
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1917
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_platon_squeeze_details
;
;
_refine_diff_density_max         2.179
_refine_diff_density_min         -1.830
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         1217
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.2412
_refine_ls_R_factor_gt           0.1996
_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)+(0.0500P)²+100.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3387
_refine_ls_wR_factor_ref         0.3579
_reflns_number_gt                876
_reflns_number_total             1217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4018536_si_001.cif
_cod_data_source_block           bbb
_cod_original_cell_volume        7024.7(17)
_cod_database_code               4336593
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
Hf1 Hf 0.43255(7) 0.43255(7) 0.43255(7) 0.206(2) Uani 1 6 d SD
Co2 Co 0.0000 0.5000 0.0000 0.268(13) Uani 1 16 d S
N1 N 0.0000 0.5000 0.1126(10) 0.276(9) Uani 1 4 d SD
C7 C 0.05859(16) 0.5000 0.1546(10) 0.276(9) Uani 1 2 d SD
C6 C 0.1331(4) 0.5000 0.1331(4) 0.276(9) Uani 1 4 d SD
C8 C 0.0357(2) 0.5000 0.2245(10) 0.276(9) Uani 1 2 d SD
H8A H 0.0649 0.5000 0.2647 0.331 Uiso 1 2 calc SR
C5 C 0.1888(4) 0.5000 0.1888(4) 0.276(9) Uani 1 4 d SD
C4 C 0.2146(4) 0.43721(10) 0.2146(4) 0.276(9) Uani 1 2 d SD
H4A H 0.1970 0.3942 0.1970 0.331 Uiso 1 2 calc SR
C2 C 0.2916(4) 0.5000 0.2916(4) 0.276(9) Uani 1 4 d SD
C1 C 0.3473(4) 0.5000 0.3473(4) 0.276(9) Uani 1 4 d SD
C3 C 0.2659(4) 0.43721(10) 0.2659(4) 0.276(9) Uani 1 2 d SD
H3A H 0.2834 0.3942 0.2834 0.331 Uiso 1 2 calc SR
O1 O 0.3750(5) 0.4562(6) 0.3750(5) 0.276(9) Uani 1 2 d SD
O1S O 0.5000 0.5000 0.3435(3) 0.276(9) Uani 1 8 d SD
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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
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 Hf1 O1 85.3(7) 5 9
O1 Hf1 O1 85.3(7) 5 .
O1 Hf1 O1 85.3(7) 9 .
O1 Hf1 O1S 75.1(2) 5 5
O1 Hf1 O1S 153.2(5) 9 5
O1 Hf1 O1S 75.1(2) . 5
O1 Hf1 O1S 153.2(5) 5 .
O1 Hf1 O1S 75.1(2) 9 .
O1 Hf1 O1S 75.1(2) . .
O1S Hf1 O1S 115.99(7) 5 .
O1 Hf1 O1S 75.1(2) 5 9
O1 Hf1 O1S 75.1(2) 9 9
O1 Hf1 O1S 153.2(5) . 9
O1S Hf1 O1S 115.99(7) 5 9
O1S Hf1 O1S 115.99(7) . 9
O1 Hf1 C1 94.9(3) 5 .
O1 Hf1 C1 94.9(3) 9 .
O1 Hf1 C1 13.0(5) . .
O1S Hf1 C1 69.25(7) 5 .
O1S Hf1 C1 69.25(8) . .
O1S Hf1 C1 166.19(19) 9 .
O1 Hf1 C1 13.0(5) 5 5
O1 Hf1 C1 94.9(3) 9 5
O1 Hf1 C1 94.9(3) . 5
O1S Hf1 C1 69.25(8) 5 5
O1S Hf1 C1 166.19(19) . 5
O1S Hf1 C1 69.25(8) 9 5
C1 Hf1 C1 102.80(16) . 5
O1 Hf1 C1 94.9(3) 5 9
O1 Hf1 C1 13.0(5) 9 9
O1 Hf1 C1 94.9(3) . 9
O1S Hf1 C1 166.19(19) 5 9
O1S Hf1 C1 69.25(8) . 9
O1S Hf1 C1 69.25(8) 9 9
C1 Hf1 C1 102.80(16) . 9
C1 Hf1 C1 102.80(16) 5 9
O1 Hf1 Hf1 132.76(12) 5 28_655
O1 Hf1 Hf1 73.8(5) 9 28_655
O1 Hf1 Hf1 132.76(12) . 28_655
O1S Hf1 Hf1 133.02(11) 5 28_655
O1S Hf1 Hf1 58.87(6) . 28_655
O1S Hf1 Hf1 58.87(6) 9 28_655
C1 Hf1 Hf1 128.11(6) . 28_655
C1 Hf1 Hf1 128.11(6) 5 28_655
C1 Hf1 Hf1 60.79(13) 9 28_655
O1 Hf1 Hf1 73.8(5) 5 26_556
O1 Hf1 Hf1 132.76(12) 9 26_556
O1 Hf1 Hf1 132.76(12) . 26_556
O1S Hf1 Hf1 58.87(6) 5 26_556
O1S Hf1 Hf1 133.02(11) . 26_556
O1S Hf1 Hf1 58.87(6) 9 26_556
C1 Hf1 Hf1 128.11(6) . 26_556
C1 Hf1 Hf1 60.79(13) 5 26_556
C1 Hf1 Hf1 128.11(6) 9 26_556
Hf1 Hf1 Hf1 89.997(1) 28_655 26_556
O1 Hf1 Hf1 132.76(12) 5 27_565
O1 Hf1 Hf1 132.76(12) 9 27_565
O1 Hf1 Hf1 73.8(5) . 27_565
O1S Hf1 Hf1 58.87(6) 5 27_565
O1S Hf1 Hf1 58.87(6) . 27_565
O1S Hf1 Hf1 133.02(11) 9 27_565
C1 Hf1 Hf1 60.78(13) . 27_565
C1 Hf1 Hf1 128.11(6) 5 27_565
C1 Hf1 Hf1 128.11(6) 9 27_565
Hf1 Hf1 Hf1 90.0 28_655 27_565
Hf1 Hf1 Hf1 90.0 26_556 27_565
N1 Co2 N1 180.0 45_565 21
N1 Co2 N1 90.000(1) 45_565 25_565
N1 Co2 N1 90.000(1) 21 25_565
N1 Co2 N1 90.000(1) 45_565 .
N1 Co2 N1 90.000(1) 21 .
N1 Co2 N1 180.000(1) 25_565 .
C7 N1 C7 108.8(4) . 2_565
C7 N1 Co2 125.6(9) . .
C7 N1 Co2 125.6(9) 2_565 .
N1 C7 C6 128.4(8) . .
N1 C7 C8 107.5(4) . .
C6 C7 C8 124.1(8) . .
C7 C6 C7 122.0(16) . 22_565
C7 C6 C5 119.0(8) . .
C7 C6 C5 119.0(8) 22_565 .
C8 C8 C7 108.1(2) 2_565 .
C4 C5 C4 119.8(2) 27_565 .
C4 C5 C6 120.09(11) 27_565 .
C4 C5 C6 120.09(11) . .
C3 C4 C5 120.09(13) . .
C3 C2 C3 119.8(2) 27_565 .
C3 C2 C1 120.10(11) 27_565 .
C3 C2 C1 120.10(11) . .
O1 C1 O1 96.2(13) . 27_565
O1 C1 C2 131.9(7) . .
O1 C1 C2 131.9(7) 27_565 .
O1 C1 Hf1 77.3(7) . 27_565
O1 C1 Hf1 18.9(7) 27_565 27_565
C2 C1 Hf1 150.78(14) . 27_565
O1 C1 Hf1 18.9(7) . .
O1 C1 Hf1 77.3(7) 27_565 .
C2 C1 Hf1 150.78(13) . .
Hf1 C1 Hf1 58.4(3) 27_565 .
C4 C3 C2 120.10(13) . .
C1 O1 Hf1 148.1(11) . .
C1 O1 O1 41.9(7) . 27_565
Hf1 O1 O1 106.2(5) . 27_565
C1 O1 Hf1 78.1(8) . 27_565
Hf1 O1 Hf1 70.0(5) . 27_565
O1 O1 Hf1 36.2(2) 27_565 27_565
Hf1 O1S Hf1 62.25(12) 2_665 28_655
Hf1 O1S Hf1 62.26(12) 2_665 27_565
Hf1 O1S Hf1 94.0(2) 28_655 27_565
Hf1 O1S Hf1 94.0(2) 2_665 .
Hf1 O1S Hf1 62.26(12) 28_655 .
Hf1 O1S Hf1 62.26(12) 27_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hf1 O1 1.622(12) 5
Hf1 O1 1.622(12) 9
Hf1 O1 1.623(12) .
Hf1 O1S 2.499(4) 5
Hf1 O1S 2.499(4) .
Hf1 O1S 2.499(4) 9
Hf1 C1 2.647(10) .
Hf1 C1 2.647(11) 5
Hf1 C1 2.647(10) 9
Hf1 Hf1 2.584(3) 28_655
Hf1 Hf1 2.584(3) 26_556
Hf1 Hf1 2.584(3) 27_565
Co2 N1 2.157(19) 45_565
Co2 N1 2.157(19) 21
Co2 N1 2.157(19) 25_565
Co2 N1 2.157(19) .
N1 C7 1.3800(7) .
N1 C7 1.3800(7) 2_565
C7 C6 1.486(8) .
C7 C8 1.4101(10) .
C6 C7 1.486(8) 22_565
C6 C5 1.5081(10) .
C8 C8 1.369(9) 2_565
C5 C4 1.3898(10) 27_565
C5 C4 1.3898(10) .
C4 C3 1.3897(10) .
C2 C3 1.3899(10) 27_565
C2 C3 1.3899(10) .
C2 C1 1.5075(10) .
C1 O1 1.126(5) .
C1 O1 1.126(5) 27_565
C1 Hf1 2.647(10) 27_565
O1 O1 1.68(2) 27_565
O1 Hf1 2.639(14) 27_565
O1S Hf1 2.499(4) 2_665
O1S Hf1 2.499(4) 28_655
O1S Hf1 2.499(4) 27_565
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 -0.008 -0.003 -0.003 4664 2094 ' '
