#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:23:47 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179576 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/41/4504120.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_4504120
loop_
_publ_author_name
'Fang, Qian-Rong'
'Zhu, Guang-Shan'
'Jin, Zhao'
'Xue, Ming'
'Wei, Xiao'
'Wang, De-Jun'
'Qiu, Shi-Lun'
_publ_section_title
;
 A Novel Metal−Organic Framework with the Diamondoid Topology
 Constructed from Pentanuclear Zinc−Carboxylate Clusters
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1035
_journal_paper_doi               10.1021/cg060829a
_journal_volume                  7
_journal_year                    2007
_chemical_formula_moiety         'C66 H56 N2 O24 Zn5'
_chemical_formula_sum            'C66 H56 N2 O24 Zn5'
_chemical_formula_weight         1587.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 109.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.829(3)
_cell_length_b                   40.672(8)
_cell_length_c                   18.528(4)
_cell_measurement_temperature    293(2)
_cell_volume                     9085(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.00cm
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.1168
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23844
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7994
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1604
_refine_ls_R_factor_gt           0.0934
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1263P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2548
_refine_ls_wR_factor_ref         0.2773
_reflns_number_gt                3671
_reflns_number_total             7994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060829asi20061122_044527.cif
_cod_data_source_block           squeezed
_cod_original_cell_volume        9086(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4504120
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
Zn1 Zn 1.0000 0.097209(18) 0.7500 0.0591(2) Uani 1 2 d S
Zn2 Zn 1.07571(4) 0.095913(13) 0.59377(3) 0.06108(17) Uani 1 1 d .
Zn3 Zn 0.89601(4) 0.151470(12) 0.60360(3) 0.06311(17) Uani 1 1 d .
N1 N 1.1063(4) 0.03411(12) 0.4201(3) 0.1060(19) Uani 1 1 d .
O1 O 0.9146(2) 0.07816(7) 0.54300(17) 0.0692(11) Uani 1 1 d .
O2 O 0.7930(2) 0.11942(7) 0.53677(17) 0.0712(11) Uani 1 1 d .
O3 O 1.0562(3) 0.13526(8) 0.51550(18) 0.0973(12) Uani 1 1 d .
O4 O 0.9639(3) 0.17746(8) 0.54078(19) 0.0868(12) Uani 1 1 d .
O5 O 0.1348(2) -0.07150(8) 0.29068(17) 0.0754(11) Uani 1 1 d .
O6 O 0.1243(2) -0.05545(7) 0.17323(16) 0.0713(11) Uani 1 1 d .
O7 O 1.3007(4) 0.30901(10) 0.1203(2) 0.1386(16) Uani 1 1 d .
O8 O 1.3361(4) 0.34354(12) 0.2064(3) 0.1723(19) Uani 1 1 d U
O9 O 1.0261(2) 0.12454(7) 0.66875(15) 0.0608(9) Uani 1 1 d .
O10 O 1.2376(3) 0.11310(11) 0.6456(3) 0.141(2) Uani 1 1 d D
O11 O 1.1290(3) 0.06855(8) 0.51857(18) 0.0844(12) Uani 1 1 d .
O12 O 0.5630(10) 0.2040(3) 0.4105(7) 0.211(6) Uani 0.50 1 d P
O13 O 0.8173(9) 0.1163(3) 0.3011(7) 0.184(3) Uani 0.50 1 d PU
C1 C 0.8171(4) 0.09090(11) 0.5227(2) 0.0626(15) Uani 1 1 d .
C2 C 0.7241(3) 0.06964(11) 0.4764(2) 0.0628(15) Uani 1 1 d .
C3 C 0.7412(3) 0.03600(11) 0.4672(2) 0.0649(15) Uani 1 1 d .
H3A H 0.8123 0.0273 0.4877 0.078 Uiso 1 1 calc R
C4 C 0.6529(3) 0.01558(12) 0.4277(3) 0.0703(16) Uani 1 1 d .
H4A H 0.6642 -0.0069 0.4245 0.084 Uiso 1 1 calc R
C5 C 0.5468(4) 0.02900(13) 0.3929(2) 0.0721(16) Uani 1 1 d .
C6 C 0.5307(4) 0.06310(13) 0.4007(3) 0.0823(19) Uani 1 1 d .
H6A H 0.4605 0.0721 0.3773 0.099 Uiso 1 1 calc R
C7 C 0.6160(4) 0.08315(13) 0.4420(3) 0.0777(18) Uani 1 1 d .
H7A H 0.6035 0.1054 0.4474 0.093 Uiso 1 1 calc R
C8 C 0.4498(4) 0.00732(12) 0.3538(2) 0.0678(16) Uani 1 1 d .
C9 C 0.4282(4) -0.02178(14) 0.3908(3) 0.0866(19) Uani 1 1 d .
H9A H 0.4769 -0.0281 0.4388 0.104 Uiso 1 1 calc R
C10 C 0.3372(4) -0.03973(13) 0.3554(3) 0.0839(18) Uani 1 1 d .
H10A H 0.3213 -0.0575 0.3814 0.101 Uiso 1 1 calc R
C11 C 0.2643(3) -0.03273(12) 0.2800(2) 0.0662(15) Uani 1 1 d .
C12 C 0.2858(4) -0.00628(12) 0.2438(2) 0.0768(17) Uani 1 1 d .
H12A H 0.2398 -0.0017 0.1939 0.092 Uiso 1 1 calc R
C13 C 0.3755(4) 0.01443(13) 0.2794(3) 0.0796(18) Uani 1 1 d .
H13A H 0.3864 0.0331 0.2538 0.096 Uiso 1 1 calc R
C14 C 0.1668(3) -0.05496(10) 0.2435(3) 0.0610(15) Uani 1 1 d .
C15 C 1.0282(4) 0.16490(12) 0.5104(3) 0.0762(16) Uani 1 1 d .
C16 C 1.0634(4) 0.18666(12) 0.4613(3) 0.0799(18) Uani 1 1 d .
C17 C 1.1279(6) 0.17523(18) 0.4182(4) 0.139(2) Uani 1 1 d U
H17A H 1.1471 0.1531 0.4201 0.166 Uiso 1 1 calc R
C18 C 1.1641(6) 0.19732(19) 0.3716(4) 0.150(2) Uani 1 1 d U
H18A H 1.2033 0.1890 0.3417 0.179 Uiso 1 1 calc R
C19 C 1.1429(4) 0.23046(12) 0.3695(3) 0.0819(18) Uani 1 1 d .
C20 C 1.0895(5) 0.24048(16) 0.4158(4) 0.129(2) Uani 1 1 d .
H20A H 1.0810 0.2629 0.4219 0.155 Uiso 1 1 calc R
C21 C 1.0461(5) 0.21828(15) 0.4556(4) 0.113(2) Uani 1 1 d U
H21A H 1.0004 0.2269 0.4805 0.135 Uiso 1 1 calc R
C22 C 1.1846(5) 0.25039(12) 0.3235(3) 0.098(2) Uani 1 1 d .
C23 C 1.1751(6) 0.24301(18) 0.2479(4) 0.135(2) Uani 1 1 d U
H23A H 1.1434 0.2230 0.2275 0.162 Uiso 1 1 calc R
C24 C 1.2120(5) 0.26474(15) 0.1996(4) 0.114(2) Uani 1 1 d U
H24A H 1.2003 0.2594 0.1486 0.137 Uiso 1 1 calc R
C25 C 1.2634(4) 0.29265(13) 0.2302(3) 0.0973(19) Uani 1 1 d .
C26 C 1.2686(6) 0.3029(2) 0.3033(5) 0.160(3) Uani 1 1 d U
H26A H 1.2946 0.3236 0.3220 0.192 Uiso 1 1 calc R
C27 C 1.2309(6) 0.2793(2) 0.3497(4) 0.161(3) Uani 1 1 d U
H27A H 1.2401 0.2849 0.4002 0.193 Uiso 1 1 calc R
C28 C 1.3026(5) 0.31573(13) 0.1826(4) 0.102(2) Uani 1 1 d .
C29 C 1.0789(4) 0.04888(14) 0.4786(3) 0.094(2) Uani 1 1 d .
H29A H 1.0139 0.0420 0.4855 0.113 Uiso 1 1 calc R
C30 C 1.2084(5) 0.04324(18) 0.4037(4) 0.150(3) Uani 1 1 d .
H30A H 1.2478 0.0600 0.4389 0.225 Uiso 1 1 calc R
H30B H 1.1882 0.0514 0.3521 0.225 Uiso 1 1 calc R
H30C H 1.2549 0.0242 0.4094 0.225 Uiso 1 1 calc R
C31 C 1.0333(7) 0.00743(18) 0.3673(4) 0.171(4) Uani 1 1 d .
H31A H 0.9697 0.0033 0.3821 0.256 Uiso 1 1 calc R
H31B H 1.0754 -0.0125 0.3721 0.256 Uiso 1 1 calc R
H31C H 1.0094 0.0149 0.3150 0.256 Uiso 1 1 calc R
C32 C 1.3053(6) 0.1145(3) 0.6177(6) 0.289(4) Uani 1 1 d DU
H32A H 1.2596 0.1246 0.5699 0.347 Uiso 1 1 calc R
H32B H 1.3048 0.0914 0.6048 0.347 Uiso 1 1 calc R
C33 C 1.4148(8) 0.1226(4) 0.6104(8) 0.360(4) Uani 1 1 d DU
H33A H 1.4322 0.1066 0.5781 0.540 Uiso 1 1 calc R
H33B H 1.4713 0.1224 0.6603 0.540 Uiso 1 1 calc R
H33C H 1.4114 0.1441 0.5881 0.540 Uiso 1 1 calc R
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'
Zn Zn 0.2839 1.4301 '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
O5 Zn1 O5 114.75(19) 6_656 5_656
O5 Zn1 O9 103.70(13) 6_656 .
O5 Zn1 O9 111.44(12) 5_656 .
O5 Zn1 O9 111.45(12) 6_656 2_756
O5 Zn1 O9 103.70(13) 5_656 2_756
O9 Zn1 O9 112.07(17) . 2_756
O10 Zn2 O9 89.34(16) . .
O10 Zn2 O11 89.10(17) . .
O9 Zn2 O11 178.04(13) . .
O10 Zn2 O1 179.19(16) . .
O9 Zn2 O1 90.75(12) . .
O11 Zn2 O1 90.83(13) . .
O10 Zn2 O3 85.88(16) . .
O9 Zn2 O3 92.46(13) . .
O11 Zn2 O3 86.23(14) . .
O1 Zn2 O3 94.93(12) . .
O10 Zn2 O6 86.06(15) . 6_656
O9 Zn2 O6 93.13(12) . 6_656
O11 Zn2 O6 87.96(13) . 6_656
O1 Zn2 O6 93.13(12) . 6_656
O3 Zn2 O6 170.13(14) . 6_656
O2 Zn3 O4 108.66(14) . .
O2 Zn3 O9 104.94(12) . .
O4 Zn3 O9 101.61(13) . .
O2 Zn3 O7 107.44(15) . 8_456
O4 Zn3 O7 94.17(16) . 8_456
O9 Zn3 O7 136.91(13) . 8_456
O2 Zn3 O8 103.76(16) . 8_456
O4 Zn3 O8 141.28(16) . 8_456
O9 Zn3 O8 89.69(14) . 8_456
O7 Zn3 O8 55.56(16) 8_456 8_456
O2 Zn3 C28 111.12(16) . 8_456
O4 Zn3 C28 116.34(17) . 8_456
O9 Zn3 C28 113.21(15) . 8_456
O7 Zn3 C28 27.09(17) 8_456 8_456
O8 Zn3 C28 28.85(17) 8_456 8_456
C29 N1 C30 121.8(5) . .
C29 N1 C31 122.6(6) . .
C30 N1 C31 115.6(6) . .
C1 O1 Zn2 135.0(3) . .
C1 O2 Zn3 125.8(3) . .
C15 O3 Zn2 138.0(3) . .
C15 O4 Zn3 122.3(3) . .
C14 O5 Zn1 118.1(3) . 5_656
C14 O6 Zn2 131.1(3) . 6_455
C28 O7 Zn3 98.5(4) . 8
C28 O8 Zn3 87.6(4) . 8
Zn1 O9 Zn3 115.93(14) . .
Zn1 O9 Zn2 111.28(13) . .
Zn3 O9 Zn2 106.55(12) . .
C32 O10 Zn2 126.4(6) . .
C29 O11 Zn2 125.2(4) . .
O2 C1 O1 126.8(4) . .
O2 C1 C2 116.9(4) . .
O1 C1 C2 116.3(4) . .
C3 C2 C7 119.3(4) . .
C3 C2 C1 120.6(4) . .
C7 C2 C1 120.1(4) . .
C4 C3 C2 120.7(4) . .
C3 C4 C5 119.8(5) . .
C6 C5 C4 119.1(4) . .
C6 C5 C8 120.0(4) . .
C4 C5 C8 120.6(5) . .
C7 C6 C5 121.5(4) . .
C6 C7 C2 119.4(5) . .
C13 C8 C9 117.2(4) . .
C13 C8 C5 121.7(4) . .
C9 C8 C5 121.1(4) . .
C10 C9 C8 119.4(4) . .
C9 C10 C11 122.9(5) . .
C12 C11 C10 118.2(4) . .
C12 C11 C14 122.5(4) . .
C10 C11 C14 119.3(4) . .
C11 C12 C13 121.6(4) . .
C12 C13 C8 120.7(5) . .
O6 C14 O5 125.9(4) . .
O6 C14 C11 119.1(4) . .
O5 C14 C11 114.9(4) . .
O3 C15 O4 125.0(5) . .
O3 C15 C16 119.5(5) . .
O4 C15 C16 115.3(4) . .
C21 C16 C17 113.3(6) . .
C21 C16 C15 125.0(6) . .
C17 C16 C15 121.6(5) . .
C18 C17 C16 120.6(7) . .
C19 C18 C17 122.2(7) . .
C20 C19 C18 115.0(6) . .
C20 C19 C22 126.8(5) . .
C18 C19 C22 118.0(6) . .
C19 C20 C21 121.9(6) . .
C16 C21 C20 126.4(7) . .
C27 C22 C23 115.5(6) . .
C27 C22 C19 120.1(6) . .
C23 C22 C19 124.3(5) . .
C22 C23 C24 123.7(6) . .
C25 C24 C23 118.3(6) . .
C24 C25 C26 121.1(6) . .
C24 C25 C28 120.1(5) . .
C26 C25 C28 118.3(6) . .
C25 C26 C27 117.1(7) . .
C22 C27 C26 123.7(7) . .
O7 C28 O8 116.7(6) . .
O7 C28 C25 122.4(5) . .
O8 C28 C25 120.8(6) . .
O7 C28 Zn3 54.4(3) . 8
O8 C28 Zn3 63.5(4) . 8
C25 C28 Zn3 170.4(4) . 8
O11 C29 N1 125.5(6) . .
O10 C32 C33 158.0(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O5 1.939(3) 6_656
Zn1 O5 1.940(3) 5_656
Zn1 O9 1.990(3) .
Zn1 O9 1.990(3) 2_756
Zn2 O10 2.088(4) .
Zn2 O9 2.072(3) .
Zn2 O11 2.073(4) .
Zn2 O1 2.085(3) .
Zn2 O3 2.116(3) .
Zn2 O6 2.153(3) 6_656
Zn3 O2 1.965(3) .
Zn3 O4 1.981(4) .
Zn3 O9 2.016(3) .
Zn3 O7 2.105(4) 8_456
Zn3 O8 2.294(6) 8_456
Zn3 C28 2.561(7) 8_456
N1 C29 1.385(8) .
N1 C30 1.489(9) .
N1 C31 1.544(8) .
O1 C1 1.286(5) .
O2 C1 1.250(5) .
O3 C15 1.252(6) .
O4 C15 1.256(6) .
O5 C14 1.277(6) .
O5 Zn1 1.939(3) 5_656
O6 C14 1.228(5) .
O6 Zn2 2.153(3) 6_455
O7 C28 1.179(8) .
O7 Zn3 2.105(4) 8
O8 C28 1.237(7) .
O8 Zn3 2.294(6) 8
O10 C32 1.154(10) .
O11 C29 1.130(6) .
C1 C2 1.486(6) .
C2 C3 1.405(6) .
C2 C7 1.423(6) .
C3 C4 1.393(6) .
C4 C5 1.401(6) .
C5 C6 1.417(7) .
C5 C8 1.495(6) .
C6 C7 1.369(6) .
C8 C13 1.412(6) .
C8 C9 1.442(7) .
C9 C10 1.342(7) .
C10 C11 1.419(6) .
C11 C12 1.345(7) .
C11 C14 1.503(6) .
C12 C13 1.396(6) .
C15 C16 1.448(7) .
C16 C21 1.303(8) .
C16 C17 1.411(9) .
C17 C18 1.428(10) .
C18 C19 1.373(9) .
C19 C20 1.331(9) .
C19 C22 1.408(8) .
C20 C21 1.396(9) .
C22 C27 1.332(9) .
C22 C23 1.396(9) .
C23 C24 1.448(10) .
C24 C25 1.337(8) .
C25 C26 1.397(10) .
C25 C28 1.488(8) .
C26 C27 1.475(11) .
C28 Zn3 2.561(7) 8
C32 C33 1.494(12) .
