#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:07:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179468 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/65/4336594.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_4336594
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 Cu3 N12 O30 Zr8'
_chemical_formula_sum            'C144 H72 Cu3 N12 O30 Zr8'
_chemical_formula_weight         3370.52
_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                   19.51(3)
_cell_length_b                   19.51(3)
_cell_length_c                   19.51(3)
_cell_measurement_temperature    173(2)
_cell_volume                     7426(2)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.2574
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67300
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_correction_T_min  0.9041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.754
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1667
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         2.361
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.409
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1350
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.640
_refine_ls_R_factor_all          0.2450
_refine_ls_R_factor_gt           0.1924
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4359
_refine_ls_wR_factor_ref         0.4573
_reflns_number_gt                728
_reflns_number_total             1350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4018536_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        7424(21)
_cod_database_code               4336594
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-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
Cu1 Cu 0.5000 0.0000 0.5000 0.085(2) Uani 1 16 d SDU
Zr1 Zr 0.93107(8) -0.06893(8) 0.06893(8) 0.177(3) Uani 1 6 d SDU
C1 C 0.8379(6) 0.0000 0.1621(6) 0.174(11) Uani 1 4 d SDU
C6 C 0.6284(4) 0.0000 0.3716(4) 0.117(8) Uani 1 4 d SDU
C5 C 0.6831(4) 0.0000 0.3169(4) 0.100(7) Uani 1 4 d SDU
C7 C 0.5573(2) 0.0000 0.3603(7) 0.137(7) Uani 1 2 d SDU
C8 C 0.5347(3) 0.0000 0.2914(7) 0.150(9) Uani 1 2 d SDU
H8A H 0.5636 0.0000 0.2515 0.180 Uiso 1 2 d SR
C3 C 0.7578(5) -0.0605(3) 0.2422(5) 0.161(9) Uani 1 2 d SDU
H3A H 0.7749 -0.1028 0.2251 0.193 Uiso 1 2 calc SR
N1 N 0.5000 0.0000 0.3996(7) 0.091(6) Uani 1 4 d SDU
C4 C 0.7085(5) -0.0607(3) 0.2915(5) 0.146(8) Uani 1 2 d SDU
H4A H 0.6915 -0.1030 0.3085 0.176 Uiso 1 2 calc SR
C2 C 0.7832(5) 0.0000 0.2168(5) 0.170(11) Uani 1 4 d SDU
O1 O 0.8581(6) -0.0571(3) 0.1419(6) 0.223(10) Uani 1 2 d SDU
O2 O 1.0000 -0.117(3) 0.0000 0.211(14) Uani 1 8 d SDU
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'
Zr Zr -2.9673 0.5597 '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
N1 Cu1 N1 180.000(1) 32_655 8_556
N1 Cu1 N1 90.000(1) 32_655 25_656
N1 Cu1 N1 90.000(1) 8_556 25_656
N1 Cu1 N1 90.000(1) 32_655 .
N1 Cu1 N1 90.000(1) 8_556 .
N1 Cu1 N1 180.000(1) 25_656 .
O1 Zr1 O1 70.5(3) 17_645 18_656
O1 Zr1 O1 70.5(3) 17_645 .
O1 Zr1 O1 70.5(3) 18_656 .
O1 Zr1 O2 93.7(11) 17_645 .
O1 Zr1 O2 93.7(11) 18_656 .
O1 Zr1 O2 160.4(14) . .
O1 Zr1 O2 160.4(14) 17_645 29_755
O1 Zr1 O2 93.7(11) 18_656 29_755
O1 Zr1 O2 93.7(11) . 29_755
O2 Zr1 O2 99.0(18) . 29_755
O1 Zr1 O2 93.7(11) 17_645 26_665
O1 Zr1 O2 160.4(14) 18_656 26_665
O1 Zr1 O2 93.7(11) . 26_665
O2 Zr1 O2 99.0(18) . 26_665
O2 Zr1 O2 99.0(18) 29_755 26_665
O1 Zr1 Zr1 134.63(2) 17_645 4_665
O1 Zr1 Zr1 134.63(2) 18_656 4_665
O1 Zr1 Zr1 83.45(18) . 4_665
O2 Zr1 Zr1 116.1(14) . 4_665
O2 Zr1 Zr1 50.6(6) 29_755 4_665
O2 Zr1 Zr1 50.6(6) 26_665 4_665
O1 Zr1 Zr1 83.45(18) 17_645 27
O1 Zr1 Zr1 134.63(2) 18_656 27
O1 Zr1 Zr1 134.63(2) . 27
O2 Zr1 Zr1 50.6(6) . 27
O2 Zr1 Zr1 116.1(14) 29_755 27
O2 Zr1 Zr1 50.6(6) 26_665 27
Zr1 Zr1 Zr1 90.0 4_665 27
O1 Zr1 Zr1 134.63(2) 17_645 2_645
O1 Zr1 Zr1 83.45(18) 18_656 2_645
O1 Zr1 Zr1 134.63(2) . 2_645
O2 Zr1 Zr1 50.6(6) . 2_645
O2 Zr1 Zr1 50.6(6) 29_755 2_645
O2 Zr1 Zr1 116.1(14) 26_665 2_645
Zr1 Zr1 Zr1 90.0 4_665 2_645
Zr1 Zr1 Zr1 90.0 27 2_645
O1 C1 O1 126.8(16) . 33
O1 C1 C2 116.6(8) . .
O1 C1 C2 116.6(8) 33 .
C7 C6 C7 108.1(15) 47_656 .
C7 C6 C5 126.0(8) 47_656 .
C7 C6 C5 126.0(7) . .
C4 C5 C4 118.7(7) . 33
C4 C5 C6 120.7(3) . .
C4 C5 C6 120.7(3) 33 .
N1 C7 C6 136.5(9) . .
N1 C7 C8 106.3(5) . 33
C6 C7 C8 117.2(8) . 33
N1 C7 C8 106.3(5) . .
C6 C7 C8 117.2(8) . .
C8 C7 C8 0.0(6) 33 .
C8 C8 C8 0(10) 33 3_655
C8 C8 C7 0(10) 33 .
C8 C8 C7 108.1(3) 3_655 .
C8 C8 H8A 0.0 33 .
C8 C8 H8A 126.0 3_655 .
C7 C8 H8A 125.9 . .
C4 C3 C2 120.8(4) . .
C4 C3 H3A 119.6 . .
C2 C3 H3A 119.6 . .
C7 N1 C7 111.1(7) 3_655 .
C7 N1 Cu1 124.4(3) 3_655 .
C7 N1 Cu1 124.4(3) . .
C3 C4 C5 120.6(4) . .
C3 C4 H4A 119.7 . .
C5 C4 H4A 119.7 . .
C3 C2 C3 118.7(7) 33 .
C3 C2 C1 120.7(3) 33 .
C3 C2 C1 120.7(3) . .
C1 O1 Zr1 123.2(9) . .
Zr1 O2 Zr1 78.8(11) . 2_645
Zr1 O2 Zr1 78.8(11) . 27
Zr1 O2 Zr1 128(3) 2_645 27
Zr1 O2 Zr1 128(3) . 28_645
Zr1 O2 Zr1 78.8(11) 2_645 28_645
Zr1 O2 Zr1 78.8(11) 27 28_645
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.958(14) 32_655
Cu1 N1 1.958(14) 8_556
Cu1 N1 1.958(14) 25_656
Cu1 N1 1.958(14) .
Zr1 O1 2.026(17) 17_645
Zr1 O1 2.026(17) 18_656
Zr1 O1 2.026(17) .
Zr1 O2 2.12(3) .
Zr1 O2 2.12(3) 29_755
Zr1 O2 2.12(3) 26_665
Zr1 Zr1 2.689(5) 4_665
Zr1 Zr1 2.689(5) 27
Zr1 Zr1 2.689(5) 2_645
C1 O1 1.245(7) .
C1 O1 1.245(7) 33
C1 C2 1.510(11) .
C6 C7 1.404(7) 47_656
C6 C7 1.404(7) .
C6 C5 1.509(11) .
C5 C4 1.376(7) .
C5 C4 1.376(7) 33
C7 N1 1.355(7) .
C7 C8 1.416(9) 33
C7 C8 1.416(9) .
C8 C8 0.00(3) 33
C8 C8 1.354(11) 3_655
C8 H8A 0.9599 .
C3 C4 1.360(8) .
C3 C2 1.373(7) .
C3 H3A 0.9500 .
N1 C7 1.355(7) 3_655
C4 H4A 0.9500 .
C2 C3 1.373(7) 33
O2 Zr1 2.12(3) 2_645
O2 Zr1 2.12(3) 27
O2 Zr1 2.12(3) 28_645
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 -0.017 -0.010 0.424 5015 2873 ' '
