#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:36:23 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179538 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/07/4500745.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_4500745
loop_
_publ_author_name
'Guo, Jingjing'
'Li, Xinhua'
'Moorefield, Charles N.'
'Newkome, George R.'
_publ_section_title
;
 Novel Twofold Interpenetrating Channel Framework Based on Metal Tetramer
 Subunits
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2695
_journal_paper_doi               10.1021/cg200242n
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C60 H96 N12 Ni4 O26'
_chemical_formula_weight         1636.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           118
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_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                   13.7327(15)
_cell_length_b                   13.7327(15)
_cell_length_c                   25.466(6)
_cell_measurement_reflns_used    2250
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      1.59
_cell_volume                     4802.6(14)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP (Bruker, 2002)'
_computing_publication_material  'SHELXL-97 (Bruker, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       'φ and ω 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  0.2038
_diffrn_reflns_av_sigmaI/netI    0.1575
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22898
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.9360
_exptl_absorpt_correction_T_min  0.8847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4077
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.1870
_refine_ls_R_factor_gt           0.1533
_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)+(0.1584P)²+19.6780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3268
_refine_ls_wR_factor_ref         0.3551
_reflns_number_gt                3090
_reflns_number_total             4077
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cg200242n_si_003.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4500745
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'-x+1/2, y+1/2, z+1/2'
'y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-y+1/2, -x+1/2, -z+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
Ni1 Ni 0.90585(12) 0.75231(15) 0.02372(9) 0.0365(6) Uani 1 1 d .
O1 O 1.0330(8) 0.7952(8) -0.0024(4) 0.046(3) Uani 1 1 d U
O2 O 1.1066(7) 0.8715(9) -0.0656(5) 0.053(3) Uani 1 1 d .
N1 N 0.8609(10) 0.7940(13) -0.0472(5) 0.055(4) Uani 1 1 d .
H1 H 0.8010 0.7947 -0.0571 2(4) Uiso 1 1 d R
N2 N 0.9678(10) 0.7004(10) 0.0887(5) 0.038(3) Uani 1 1 d .
N3 N 0.7824(9) 0.6888(8) 0.0419(4) 0.028(3) Uani 1 1 d .
C1 C 1.0349(13) 0.8335(13) -0.0492(7) 0.049(4) Uani 1 1 d U
C2 C 0.940(2) 0.817(2) -0.0799(11) 0.089(7) Uani 1 1 d U
H2 H 0.9551 0.7486 -0.0864 0.3(3) Uiso 1 1 d R
C3 C 0.941(3) 0.838(4) -0.1290(11) 0.19(3) Uani 1 1 d .
H3A H 1.0050 0.8277 -0.1428 0.07(6) Uiso 1 1 d R
H3B H 0.9222 0.9045 -0.1339 0.00(3) Uiso 1 1 d R
H3C H 0.8956 0.7962 -0.1471 0.07(7) Uiso 1 1 d R
C4 C 1.0471(11) 0.6379(11) 0.0844(5) 0.032(3) Uani 1 1 d .
H4 H 1.0683 0.6170 0.0516 0.08(6) Uiso 1 1 d R
C5 C 1.0943(18) 0.6072(17) 0.1298(7) 0.080(9) Uani 1 1 d .
H5 H 1.1532 0.5743 0.1266 0.12(9) Uiso 1 1 calc R
C6 C 1.0574(13) 0.6235(11) 0.1789(8) 0.051(5) Uani 1 1 d .
C7 C 0.9723(15) 0.6793(18) 0.1828(8) 0.076(7) Uani 1 1 d .
H7 H 0.9420 0.6936 0.2146 0.05(5) Uiso 1 1 d R
C8 C 0.9369(11) 0.7119(11) 0.1336(5) 0.030(3) Uani 1 1 d .
H8 H 0.8800 0.7485 0.1357 0.02(4) Uiso 1 1 d R
C9 C 1.1027(14) 0.5851(14) 0.2255(7) 0.057(5) Uani 1 1 d .
H9 H 1.1525 0.5406 0.2194 0.01(3) Uiso 1 1 d R
C10 C 0.7764(13) 0.5909(14) 0.0455(7) 0.053(5) Uani 1 1 d U
H10 H 0.8319 0.5544 0.0385 0.04(4) Uiso 1 1 d R
C11 C 0.6847(17) 0.5379(13) 0.0603(9) 0.073(6) Uani 1 1 d .
H11 H 0.6842 0.4716 0.0676 0.01(3) Uiso 1 1 d R
C12 C 0.6038(12) 0.5920(11) 0.0623(7) 0.047(4) Uani 1 1 d .
C13 C 0.6032(18) 0.6981(16) 0.0585(11) 0.090(8) Uani 1 1 d .
H13 H 0.5470 0.7351 0.0624 0.04(4) Uiso 1 1 calc R
C14 C 0.6942(11) 0.7389(10) 0.0485(5) 0.032(3) Uani 1 1 d .
H14 H 0.6967 0.8064 0.0458 0.02(3) Uiso 1 1 d R
H15 H 0.4466 0.5887 0.0651 0.10(8) Uiso 1 1 d R
C15 C 0.5017(15) 0.5471(14) 0.0669(6) 0.054(5) Uani 1 1 d .
O3 O 0.652(4) 0.297(4) 0.156(2) 0.106(14) Uani 0.50 1 d PU
H3G H 0.6434 0.3501 0.1397 0.158 Uiso 0.50 1 d PR
H3D H 0.7127 0.2897 0.1624 0.158 Uiso 0.50 1 d PR
O4 O 0.5000 0.5000 0.242(12) 0.43(12) Uani 0.50 2 d SPU
H4D H 0.5443 0.5247 0.2232 0.648 Uiso 0.25 1 d PR
H4C H 0.4728 0.4534 0.2260 0.648 Uiso 0.25 1 d PR
O5 O 0.167(8) 0.067(8) 0.213(4) 0.17(4) Uani 0.25 1 d PU
H5A H 0.1885 0.0084 0.2142 0.249 Uiso 0.25 1 d PR
H5C H 0.1190 0.0693 0.1921 0.249 Uiso 0.25 1 d PR
O6 O 0.867(6) 0.367(6) 0.7500 0.478(4) Uani 1 2 d SU
H6D H 0.8736 0.3855 0.7183 0.718 Uiso 0.50 1 d PR
H6C H 0.8513 0.3072 0.7506 0.718 Uiso 0.50 1 d PR
O7 O 0.616(18) 0.272(16) 0.159(9) 0.26(11) Uani 0.25 1 d PU
H7A H 0.6527 0.2249 0.1679 0.389 Uiso 0.25 1 d PR
H7B H 0.5904 0.2963 0.1869 0.389 Uiso 0.25 1 d PR
O8 O 0.673(8) 0.315(8) 0.192(5) 0.15(4) Uani 0.25 1 d PU
H8A H 0.7123 0.2734 0.2049 0.221 Uiso 0.25 1 d PR
H8B H 0.6430 0.3432 0.2174 0.221 Uiso 0.25 1 d PR
O9 O 0.658(2) 0.281(2) 0.1068(12) 0.071(8) Uani 0.50 1 d PU
H9A H 0.7194 0.2720 0.1091 0.107 Uiso 0.50 1 d PR
H9C H 0.6348 0.2442 0.0833 0.107 Uiso 0.50 1 d PR
O10 O 0.326(10) 0.337(10) 0.216(5) 0.20(5) Uani 0.25 1 d PU
H10D H 0.3728 0.3600 0.1981 0.293 Uiso 0.25 1 d PR
H10B H 0.2759 0.3717 0.2123 0.293 Uiso 0.25 1 d PR
O11 O 0.934(8) 0.495(8) 0.788(4) 0.16(4) Uani 0.25 1 d PU
H11A H 0.9884 0.5058 0.8031 0.234 Uiso 0.25 1 d PR
H11B H 0.8907 0.5316 0.8017 0.234 Uiso 0.25 1 d PR
O12 O 0.5000 0.5000 0.0000 0.276(4) Uani 1 4 d SU
H12A H 0.4459 0.4717 -0.0054 0.414 Uiso 0.25 1 d PR
H12B H 0.5068 0.5464 -0.0218 0.414 Uiso 0.25 1 d PR
O13 O 1.0000 0.5000 0.055(6) 0.29(7) Uani 0.50 2 d SPU
H13A H 1.0290 0.4946 0.0254 0.440 Uiso 0.25 1 d PR
H13B H 1.0026 0.5589 0.0650 0.440 Uiso 0.25 1 d PR
O14 O 0.216(8) 0.284(8) 0.2500 0.245(4) Uani 0.50 2 d SPU
H14A H 0.2750 0.2228 0.2339 0.00(10) Uiso 0.25 1 d PR
H14C H 0.2439 0.2539 0.2732 0.2(7) Uiso 0.25 1 d PR
O15 O 1.0000 0.5000 0.9426(10) 0.035(7) Uani 0.50 2 d SPU
H15A H 1.0358 0.5157 0.9685 0.053 Uiso 0.25 1 d PR
H15B H 0.9489 0.5350 0.9426 0.053 Uiso 0.25 1 d PR
O16 O 0.5000 0.5000 0.3378(10) 0.038(7) Uani 0.50 2 d SPU
H16B H 0.4554 0.4608 0.3472 0.057 Uiso 0.25 1 d PR
H16C H 0.4746 0.5534 0.3280 0.057 Uiso 0.25 1 d PR
O17 O 1.0000 0.5000 0.095(5) 0.21(5) Uani 0.50 2 d SPU
H17D H 0.9412 0.4831 0.0898 0.317 Uiso 0.25 1 d PR
H17C H 1.0249 0.4649 0.1187 0.317 Uiso 0.25 1 d PR
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'
Ni Ni 0.3393 1.1124 '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'
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 Ni1 N3 169.7(5) . .
O1 Ni1 N2 90.5(5) . .
N3 Ni1 N2 90.8(5) . .
O1 Ni1 N1 83.3(5) . .
N3 Ni1 N1 94.3(5) . .
N2 Ni1 N1 171.0(6) . .
O1 Ni1 O2 95.0(5) . 2_575
N3 Ni1 O2 95.1(5) . 2_575
N2 Ni1 O2 90.2(5) . 2_575
N1 Ni1 O2 96.7(6) . 2_575
C1 O1 Ni1 116.7(11) . .
C1 O2 Ni1 129.5(12) . 4_755
C2 N1 Ni1 111.3(13) . .
C2 N1 H1 124.4 . .
Ni1 N1 H1 124.3 . .
C8 N2 C4 114.9(12) . .
C8 N2 Ni1 125.4(11) . .
C4 N2 Ni1 119.3(10) . .
C10 N3 C14 115.3(13) . .
C10 N3 Ni1 120.8(11) . .
C14 N3 Ni1 123.8(9) . .
O2 C1 O1 120.9(17) . .
O2 C1 C2 126.1(18) . .
O1 C1 C2 112.9(17) . .
C3 C2 N1 129(3) . .
C3 C2 C1 117(3) . .
N1 C2 C1 113(2) . .
C3 C2 H2 92.6 . .
N1 C2 H2 92.6 . .
C1 C2 H2 92.6 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C4 N2 119.1(14) . .
C5 C4 H4 120.4 . .
N2 C4 H4 120.4 . .
C5 C4 H13B 105.9 . .
N2 C4 H13B 99.9 . .
H4 C4 H13B 64.0 . .
C6 C5 C4 122.5(17) . .
C6 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
C5 C6 C7 117.6(17) . .
C5 C6 C9 122.2(17) . .
C7 C6 C9 120.2(19) . .
C6 C7 C8 113.4(18) . .
C6 C7 H7 123.3 . .
C8 C7 H7 123.3 . .
N2 C8 C7 131.6(15) . .
N2 C8 H8 114.2 . .
C7 C8 H8 114.2 . .
C9 C9 C6 130(2) 6_545 .
C9 C9 H9 114.9 6_545 .
C6 C9 H9 114.9 . .
N3 C10 C11 123.4(16) . .
N3 C10 H10 118.3 . .
C11 C10 H10 118.3 . .
C12 C11 C10 115.9(16) . .
C12 C11 H11 122.1 . .
C10 C11 H11 122.1 . .
C11 C12 C13 123.9(19) . .
C11 C12 C15 122.5(16) . .
C13 C12 C15 113.6(16) . .
C14 C13 C12 114.1(19) . .
C14 C13 H13 122.9 . .
C12 C13 H13 122.9 . .
C13 C14 N3 126.8(15) . .
C13 C14 H14 116.6 . .
N3 C14 H14 116.6 . .
C15 C15 C12 116(2) 3_665 .
C15 C15 H15 124.9 3_665 .
C12 C15 H15 118.8 . .
H3G O3 H3D 109.5 . .
H3G O3 H7A 166.1 . .
H3D O3 H7A 80.3 . .
H3G O3 H7B 102.8 . .
H3D O3 H7B 125.0 . .
H7A O3 H7B 78.1 . .
H4D O4 H4C 109.5 . .
H5A O5 H5C 109.5 . .
H6D O6 H6C 109.6 . .
H3G O7 H3D 64.8 . .
H3G O7 H7A 126.0 . .
H3D O7 H7A 62.8 . .
H3G O7 H7B 97.3 . .
H3D O7 H7B 107.2 . .
H7A O7 H7B 109.5 . .
H3D O8 H7A 57.8 . .
H3D O8 H7B 111.2 . .
H7A O8 H7B 64.3 . .
H3D O8 H8A 72.8 . .
H7A O8 H8A 72.6 . .
H7B O8 H8A 121.1 . .
H3D O8 H8B 172.4 . .
H7A O8 H8B 129.7 . .
H7B O8 H8B 74.1 . .
H8A O8 H8B 109.5 . .
H3G O9 H9A 103.0 . .
H3G O9 H9C 147.4 . .
H9A O9 H9C 109.5 . .
H10D O10 H10B 109.5 . .
O11 O11 H11A 27.2 3_765 .
O11 O11 H11B 130.8 3_765 .
H11A O11 H11B 109.5 . .
C15 O12 C15 41.6(12) 2_565 4_655
C15 O12 C15 150.9(8) 2_565 3_665
C15 O12 C15 150.9(8) 4_655 3_665
C15 O12 H12A 98.8 2_565 .
C15 O12 H12A 62.9 4_655 .
C15 O12 H12A 88.7 3_665 .
C15 O12 H12B 50.2 2_565 .
C15 O12 H12B 54.5 4_655 .
C15 O12 H12B 151.4 3_665 .
H12A O12 H12B 109.5 . .
H13A O13 H13B 109.5 . .
H13A O13 H17D 158.8 . .
H13B O13 H17D 89.1 . .
H14A O14 H14C 66.1 . .
H15A O15 H15B 109.5 . .
H16B O16 H16C 109.5 . .
H13B O17 H17D 97.4 . .
H13B O17 H17C 153.1 . .
H17D O17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 1.959(11) .
Ni1 N3 1.961(11) .
Ni1 N2 1.991(11) .
Ni1 N1 1.994(12) .
Ni1 O2 2.262(12) 2_575
O1 C1 1.31(2) .
O2 C1 1.19(2) .
O2 Ni1 2.262(12) 4_755
N1 C2 1.40(3) .
N1 H1 0.8600 .
N2 C8 1.232(19) .
N2 C4 1.392(19) .
N3 C10 1.35(2) .
N3 C14 1.404(19) .
C1 C2 1.54(3) .
C2 C3 1.28(4) .
C2 H2 0.9800 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 C5 1.39(2) .
C4 H4 0.9300 .
C5 C6 1.37(3) .
C5 H5 0.9300 .
C6 C7 1.40(3) .
C6 C9 1.44(2) .
C7 C8 1.42(2) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 C9 1.29(4) 6_545
C9 H9 0.9300 .
C10 C11 1.50(3) .
C10 H10 0.9300 .
C11 C12 1.34(3) .
C11 H11 0.9300 .
C12 C13 1.46(3) .
C12 C15 1.54(3) .
C13 C14 1.39(3) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 C15 1.29(4) 3_665
C15 H15 0.9498 .
O3 H3G 0.8502 .
O3 H3D 0.8500 .
O3 H7A 1.0314 .
O3 H7B 1.1649 .
O4 H4D 0.8499 .
O4 H4C 0.8499 .
O5 H5A 0.8500 .
O5 H5C 0.8501 .
O6 H6D 0.8504 .
O6 H6C 0.8487 .
O7 H7A 0.8501 .
O7 H7B 0.8499 .
O8 H8A 0.8499 .
O8 H8B 0.8499 .
O9 H9A 0.8501 .
O9 H9C 0.8500 .
O10 H10D 0.8500 .
O10 H10B 0.8501 .
O11 O11 1.8(2) 3_765
O11 H11A 0.8500 .
O11 H11B 0.8499 .
O12 H12A 0.8499 .
O12 H12B 0.8500 .
O13 H13A 0.8501 .
O13 H13B 0.8500 .
O14 H14A 1.2319 .
O14 H14C 0.8133 .
O15 H15A 0.8499 .
O15 H15B 0.8500 .
O16 H16B 0.8500 .
O16 H16C 0.8501 .
O17 H17D 0.8500 .
O17 H17C 0.8498 .
