#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:36:23 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179538 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/07/4500744.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_4500744
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 H86 Cu4 N12 O21'
_chemical_formula_weight         1565.57
_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                   13.7561(3)
_cell_length_b                   13.7561(3)
_cell_length_c                   25.5306(12)
_cell_measurement_reflns_used    3549
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      1.58
_cell_volume                     4831.2(3)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0838
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24023
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  0.8969
_exptl_absorpt_correction_T_min  0.8292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4221
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.1266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1088P)²+25.8159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2867
_refine_ls_wR_factor_ref         0.2888
_reflns_number_gt                4039
_reflns_number_total             4221
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cg200242n_si_002.cif
_cod_data_source_block           l061015m
_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_original_sg_symbol_H-M      P-4n2
_cod_database_code               4500744
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
Cu1 Cu 0.09339(8) 0.24926(11) 0.47627(6) 0.0395(4) Uani 1 1 d .
O1 O -0.0303(5) 0.2017(6) 0.5007(3) 0.0390(19) Uani 1 1 d .
O2 O -0.1094(5) 0.1361(7) 0.5682(3) 0.045(2) Uani 1 1 d .
N1 N 0.0304(6) 0.3016(7) 0.4108(3) 0.0329(19) Uani 1 1 d U
N2 N 0.2191(7) 0.3127(7) 0.4595(4) 0.040(2) Uani 1 1 d U
N3 N 0.1374(7) 0.2098(7) 0.5480(3) 0.039(2) Uani 1 1 d U
H3A H 0.1971 0.2027 0.5571 0.047 Uiso 1 1 calc R
C1 C -0.0395(8) 0.1711(8) 0.5487(5) 0.039(3) Uani 1 1 d .
C2 C 0.0575(9) 0.1952(10) 0.5812(4) 0.046(3) Uani 1 1 d .
H2 H 0.0461 0.2566 0.5997 0.055 Uiso 1 1 calc R
C3 C 0.0730(12) 0.1184(15) 0.6221(6) 0.085(5) Uani 1 1 d .
H3B H 0.0809 0.0563 0.6054 0.127 Uiso 1 1 calc R
H3C H 0.0177 0.1162 0.6450 0.127 Uiso 1 1 calc R
H3D H 0.1302 0.1334 0.6420 0.127 Uiso 1 1 calc R
C4 C 0.0666(12) 0.2837(11) 0.3643(5) 0.059(4) Uani 1 1 d .
H4 H 0.1214 0.2443 0.3621 0.071 Uiso 1 1 calc R
C5 C 0.0280(10) 0.3199(12) 0.3186(5) 0.062(4) Uani 1 1 d .
H5 H 0.0574 0.3068 0.2866 0.074 Uiso 1 1 calc R
C6 C -0.0568(9) 0.3773(9) 0.3210(5) 0.050(3) Uani 1 1 d .
C7 C -0.0931(12) 0.3945(10) 0.3691(7) 0.068(4) Uani 1 1 d .
H7 H -0.1485 0.4327 0.3727 0.081 Uiso 1 1 calc R
C8 C -0.0480(10) 0.3550(10) 0.4144(5) 0.049(3) Uani 1 1 d .
H8 H -0.0747 0.3673 0.4473 0.058 Uiso 1 1 calc R
C9 C -0.1042(10) 0.4170(11) 0.2745(5) 0.057(4) Uani 1 1 d .
H9 H -0.1540 0.4615 0.2800 0.069 Uiso 1 1 calc R
C10 C 0.3042(9) 0.2670(9) 0.4551(6) 0.054(4) Uani 1 1 d .
H10 H 0.3026 0.1998 0.4586 0.065 Uiso 1 1 calc R
C11 C 0.3897(10) 0.3055(12) 0.4466(7) 0.074(5) Uani 1 1 d .
H11 H 0.4450 0.2666 0.4458 0.089 Uiso 1 1 calc R
C12 C 0.3969(10) 0.4057(10) 0.4385(5) 0.051(3) Uani 1 1 d .
C13 C 0.3086(11) 0.4596(11) 0.4421(5) 0.062(4) Uani 1 1 d U
H13 H 0.3081 0.5268 0.4382 0.075 Uiso 1 1 calc R
C14 C 0.2229(10) 0.4081(10) 0.4518(5) 0.053(3) Uani 1 1 d U
H14 H 0.1649 0.4428 0.4529 0.063 Uiso 1 1 calc R
C15 C 0.4926(9) 0.4538(10) 0.4328(6) 0.058(4) Uani 1 1 d .
H15 H 0.5467 0.4139 0.4289 0.069 Uiso 1 1 calc R
O3 O 0.235(4) 0.265(4) 0.7500 0.441(4) Uani 1 2 d SU
H3E H 0.2668 0.2187 0.7580 0.662 Uiso 0.50 1 d PR
H3F H 0.2708 0.3194 0.7553 0.662 Uiso 0.50 1 d PR
O4 O 0.6681(19) 0.2901(19) 0.3919(10) 0.092(7) Uani 0.50 1 d PU
H4A H 0.7226 0.3188 0.3894 0.138 Uiso 0.50 1 d PR
H4B H 0.6726 0.2440 0.4140 0.138 Uiso 0.50 1 d PR
O5 O 0.731(6) 0.648(6) 0.303(3) 0.15(2) Uani 0.25 1 d PU
H5D H 0.7527 0.6711 0.2745 0.221 Uiso 0.25 1 d PR
H5B H 0.7664 0.6654 0.3283 0.221 Uiso 0.25 1 d PR
O6 O 0.545(7) 0.520(9) 0.278(3) 0.21(4) Uani 0.25 1 d PU
H6B H 0.5441 0.4678 0.2599 0.312 Uiso 0.25 1 d PR
H6C H 0.4994 0.5571 0.2676 0.312 Uiso 0.25 1 d PR
O7 O 0.331(8) 0.206(9) 0.301(4) 0.22(4) Uani 0.25 1 d PU
H7A H 0.3434 0.2128 0.2687 0.330 Uiso 0.25 1 d PR
H7C H 0.3289 0.1464 0.3089 0.330 Uiso 0.25 1 d PR
O8 O 0.667(6) 0.588(6) 0.293(3) 0.15(2) Uani 0.25 1 d PU
H8B H 0.6639 0.5269 0.2884 0.229 Uiso 0.25 1 d PR
H8C H 0.6096 0.6117 0.2914 0.229 Uiso 0.25 1 d PR
O9 O 1.0000 0.5000 0.5397(11) 0.069(8) Uani 0.50 2 d SPU
H9A H 0.9567 0.5381 0.5516 0.104 Uiso 0.25 1 d PR
H9C H 1.0077 0.5105 0.5071 0.104 Uiso 0.25 1 d PR
O10 O 0.471(5) 0.029(5) 0.2500 0.272(4) Uani 0.50 2 d SPU
H10D H 0.4325 0.0594 0.2734 0.408 Uiso 0.25 1 d PR
H10C H 0.4951 0.0847 0.2330 0.408 Uiso 0.25 1 d PR
O11 O 1.028(3) 0.433(3) 0.5284(16) 0.059(9) Uani 0.25 1 d PU
H11D H 1.0463 0.3802 0.5139 0.088 Uiso 0.25 1 d PR
H11A H 1.0464 0.4331 0.5602 0.088 Uiso 0.25 1 d PR
O12 O 0.523(19) 0.073(17) 0.204(9) 0.46(6) Uani 0.25 1 d PU
H12A H 0.4806 0.1096 0.2182 0.690 Uiso 0.25 1 d PR
H12B H 0.5612 0.1076 0.1855 0.690 Uiso 0.25 1 d PR
O13 O 0.659(4) 0.376(5) 0.334(2) 0.111(18) Uani 0.25 1 d PU
H13B H 0.6646 0.3440 0.3056 0.166 Uiso 0.25 1 d PR
H13C H 0.6636 0.4365 0.3274 0.166 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'
Cu Cu 0.3201 1.2651 '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 Cu1 N2 171.5(4) . .
O1 Cu1 N3 83.0(3) . .
N2 Cu1 N3 93.0(4) . .
O1 Cu1 N1 90.6(3) . .
N2 Cu1 N1 92.2(4) . .
N3 Cu1 N1 169.9(4) . .
O1 Cu1 O2 95.8(4) . 2_556
N2 Cu1 O2 92.2(4) . 2_556
N3 Cu1 O2 98.4(3) . 2_556
N1 Cu1 O2 90.0(3) . 2_556
C1 O1 Cu1 120.0(7) . .
C1 O2 Cu1 125.1(8) . 4_556
C8 N1 C4 118.8(11) . .
C8 N1 Cu1 119.8(8) . .
C4 N1 Cu1 121.4(8) . .
C14 N2 C10 114.7(10) . .
C14 N2 Cu1 120.1(9) . .
C10 N2 Cu1 125.2(8) . .
C2 N3 Cu1 110.7(7) . .
C2 N3 H3A 124.6 . .
Cu1 N3 H3A 124.6 . .
O2 C1 O1 127.2(10) . .
O2 C1 C2 122.9(11) . .
O1 C1 C2 109.8(10) . .
N3 C2 C3 114.2(12) . .
N3 C2 C1 111.7(9) . .
C3 C2 C1 109.4(11) . .
N3 C2 H2 107.1 . .
C3 C2 H2 107.1 . .
C1 C2 H2 107.1 . .
C2 C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C3 H3D 109.5 . .
H3B C3 H3D 109.5 . .
H3C C3 H3D 109.5 . .
N1 C4 C5 123.7(13) . .
N1 C4 H4 118.2 . .
C5 C4 H4 118.2 . .
C4 C5 C6 119.0(13) . .
C4 C5 H5 120.5 . .
C6 C5 H5 120.5 . .
C7 C6 C5 116.4(12) . .
C7 C6 C9 120.7(13) . .
C5 C6 C9 122.9(14) . .
C6 C7 C8 120.9(14) . .
C6 C7 H7 119.6 . .
C8 C7 H7 119.6 . .
N1 C8 C7 121.2(13) . .
N1 C8 H8 119.4 . .
C7 C8 H8 119.4 . .
C9 C9 C6 126.2(18) 6_455 .
C9 C9 H9 116.9 6_455 .
C6 C9 H9 116.9 . .
C11 C10 N2 127.9(13) . .
C11 C10 H10 116.1 . .
N2 C10 H10 116.1 . .
C10 C11 C12 119.1(14) . .
C10 C11 H11 120.5 . .
C12 C11 H11 120.5 . .
C11 C12 C13 116.3(13) . .
C11 C12 C15 121.2(12) . .
C13 C12 C15 122.1(12) . .
C14 C13 C12 117.8(13) . .
C14 C13 H13 121.1 . .
C12 C13 H13 121.1 . .
N2 C14 C13 124.1(13) . .
N2 C14 H14 118.0 . .
C13 C14 H14 118.0 . .
C15 C15 C12 125.5(16) 3_665 .
C15 C15 H15 117.2 3_665 .
C12 C15 H15 117.2 . .
H3E O3 H3F 109.3 . .
H4A O4 H4B 109.5 . .
H5D O5 H5B 109.5 . .
O6 O6 H6B 69.3 3_665 .
O6 O6 H6C 64.4 3_665 .
H6B O6 H6C 109.5 . .
H7A O7 H7C 109.5 . .
H8B O8 H8C 109.5 . .
O11 O9 H9A 44.9 3_765 .
O11 O9 H9C 68.0 3_765 .
H9A O9 H9C 109.5 . .
O11 O9 H11A 165.8 3_765 .
H9A O9 H11A 131.9 . .
H9C O9 H11A 118.5 . .
O10 O10 O12 87(10) 3_655 8
O10 O10 O12 55(8) 3_655 3_655
O12 O10 O12 99(10) 8 3_655
O10 O10 O12 55(8) 3_655 6_545
O12 O10 O12 78(10) 8 6_545
O12 O10 O12 109(10) 3_655 6_545
O10 O10 H10D 137.7 3_655 .
O12 O10 H10D 57.6 8 .
O12 O10 H10D 143.8 3_655 .
O12 O10 H10D 92.7 6_545 .
O10 O10 H10C 108.8 3_655 .
O12 O10 H10C 153.4 8 .
O12 O10 H10C 108.0 3_655 .
O12 O10 H10C 93.5 6_545 .
H10D O10 H10C 98.5 . .
O10 O10 H12A 119.9 3_655 .
O12 O10 H12A 152.2 8 .
O12 O10 H12A 103.5 3_655 .
O12 O10 H12A 109.9 6_545 .
H10D O10 H12A 94.8 . .
H10C O10 H12A 16.6 . .
H9C O11 H11D 127.9 . .
H9C O11 H11A 119.2 . .
H11D O11 H11A 109.5 . .
O10 O12 H10C 66.9 3_655 .
O10 O12 H12A 102.3 3_655 .
H10C O12 H12A 37.6 . .
O10 O12 H12B 138.7 3_655 .
H10C O12 H12B 131.2 . .
H12A O12 H12B 109.5 . .
H13B O13 H13C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.927(6) .
Cu1 N2 1.983(9) .
Cu1 N3 2.003(9) .
Cu1 N1 2.015(8) .
Cu1 O2 2.309(8) 2_556
O1 C1 1.302(13) .
O2 C1 1.184(14) .
O2 Cu1 2.309(8) 4_556
N1 C8 1.308(15) .
N1 C4 1.311(16) .
N2 C14 1.328(16) .
N2 C10 1.334(16) .
N3 C2 1.402(16) .
N3 H3A 0.8600 .
C1 C2 1.605(16) .
C2 C3 1.50(2) .
C2 H2 0.9800 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C3 H3D 0.9600 .
C4 C5 1.375(18) .
C4 H4 0.9300 .
C5 C6 1.409(19) .
C5 H5 0.9300 .
C6 C7 1.35(2) .
C6 C9 1.460(16) .
C7 C8 1.421(18) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 C9 1.32(3) 6_455
C9 H9 0.9300 .
C10 C11 1.308(19) .
C10 H10 0.9300 .
C11 C12 1.40(2) .
C11 H11 0.9300 .
C12 C13 1.43(2) .
C12 C15 1.482(18) .
C13 C14 1.397(19) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 C15 1.29(3) 3_665
C15 H15 0.9300 .
O3 H3E 0.7935 .
O3 H3F 0.9068 .
O4 H4A 0.8500 .
O4 H4B 0.8500 .
O5 H5D 0.8499 .
O5 H5B 0.8501 .
O6 O6 1.35(19) 3_665
O6 H6B 0.8500 .
O6 H6C 0.8499 .
O7 H7A 0.8499 .
O7 H7C 0.8500 .
O8 H8B 0.8500 .
O8 H8C 0.8499 .
O9 O11 1.04(4) 3_765
O9 H9A 0.8500 .
O9 H9C 0.8502 .
O9 H11A 1.2367 .
O10 O10 1.14(18) 3_655
O10 O12 1.5(2) 8
O10 O12 1.8(2) 3_655
O10 O12 1.8(2) 6_545
O10 H10D 0.8952 .
O10 H10C 0.9372 .
O10 H12A 1.3753 .
O11 H9C 1.2302 .
O11 H11D 0.8501 .
O11 H11A 0.8500 .
O12 O10 1.8(2) 3_655
O12 H10C 0.8482 .
O12 H12A 0.8500 .
O12 H12B 0.8501 .
O13 H13B 0.8500 .
O13 H13C 0.8500 .
