#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505530.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_4505530
loop_
_publ_author_name
'He, Kun-Huan'
'Song, Wei-Chao'
'Li, Yun-Wu'
'Chen, Yong-Qiang'
'Bu, Xian-He'
_publ_section_title
;
 A New 10-Connected Coordination Network with Pentanuclear Zinc Clusters
 as Secondary Building Units
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1064
_journal_paper_doi               10.1021/cg2014495
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C76 H54 N8 O18 Zn5'
_chemical_formula_weight         1694.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 117.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.309(3)
_cell_length_b                   15.799(3)
_cell_length_c                   16.424(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     3521.7(15)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  SCX-MINI
_diffrn_measurement_method       multi-scan
_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  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29856
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1720.0
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0274P)²+4.9990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                4782
_reflns_number_total             6194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2014495_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        3521.6(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4505530
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
N1 N 0.3224(2) 0.9996(2) 1.4574(2) 0.0266(8) Uani 1 1 d .
C38 C 0.3600(3) 1.0672(3) 1.4392(3) 0.0363(11) Uani 1 1 d .
H38 H 0.3517 1.1219 1.4553 0.044 Uiso 1 1 calc R
C37 C 0.3515(3) 0.9338(3) 1.4223(3) 0.0388(12) Uani 1 1 d .
H37 H 0.3362 0.8773 1.4250 0.047 Uiso 1 1 calc R
O3 O 0.1449(2) 0.58551(19) 0.9198(2) 0.0387(8) Uani 1 1 d .
O4 O 0.0091(2) 0.61213(16) 0.93306(18) 0.0272(7) Uani 1 1 d .
C6 C 0.0641(3) 0.6213(2) 0.8955(3) 0.0235(9) Uani 1 1 d .
O8 O 0.6565(2) 0.5654(2) 0.7435(2) 0.0451(9) Uani 1 1 d .
O7 O 0.6535(2) 0.5775(2) 0.8770(2) 0.0535(10) Uani 1 1 d .
C36 C 0.4057(4) 0.9629(3) 1.3833(3) 0.0449(13) Uani 1 1 d .
H36 H 0.4337 0.9307 1.3540 0.054 Uiso 1 1 calc R
N2 N 0.4118(3) 1.0480(3) 1.3945(2) 0.0357(9) Uani 1 1 d .
C35 C 0.4565(4) 1.1078(4) 1.3570(3) 0.0510(14) Uani 1 1 d .
H35A H 0.5190 1.0857 1.3650 0.061 Uiso 1 1 calc R
H35B H 0.4689 1.1610 1.3900 0.061 Uiso 1 1 calc R
C32 C 0.3893(3) 1.1228(3) 1.2563(3) 0.0403(12) Uani 1 1 d .
C33 C 0.3171(4) 1.1833(3) 1.2285(3) 0.0506(14) Uani 1 1 d .
H33 H 0.3112 1.2168 1.2722 0.061 Uiso 1 1 calc R
C34 C 0.2534(4) 1.1954(3) 1.1370(3) 0.0529(14) Uani 1 1 d .
H34 H 0.2046 1.2365 1.1197 0.063 Uiso 1 1 calc R
C31 C 0.3969(4) 1.0749(4) 1.1901(3) 0.0589(16) Uani 1 1 d .
H31 H 0.4459 1.0339 1.2078 0.071 Uiso 1 1 calc R
C30 C 0.3337(5) 1.0862(4) 1.0985(4) 0.075(2) Uani 1 1 d .
H30 H 0.3397 1.0525 1.0549 0.090 Uiso 1 1 calc R
C29 C 0.2613(4) 1.1475(4) 1.0711(3) 0.0569(16) Uani 1 1 d .
O2 O -0.1577(2) 0.88887(18) 0.5620(2) 0.0348(7) Uani 1 1 d .
Zn1 Zn 0.0000 1.0000 0.5000 0.01873(15) Uani 1 2 d S
Zn2 Zn 0.22930(4) 0.98375(3) 0.71110(3) 0.02657(13) Uani 1 1 d .
Zn3 Zn 0.22995(3) 1.00108(3) 0.51603(3) 0.02229(12) Uani 1 1 d .
O9 O 0.14974(19) 1.02031(15) 0.58538(17) 0.0212(6) Uani 1 1 d D
O1 O 0.0001(2) 0.92500(17) 0.60547(18) 0.0277(7) Uani 1 1 d .
O5 O 0.2826(2) 0.87043(18) 0.7264(2) 0.0382(8) Uani 1 1 d .
O6 O 0.3015(2) 0.89164(19) 0.6015(2) 0.0423(8) Uani 1 1 d .
C13 C 0.3140(3) 0.8503(3) 0.6693(3) 0.0302(10) Uani 1 1 d .
N4 N 0.1884(3) 1.0143(3) 0.8062(2) 0.0385(9) Uani 1 1 d .
C24 C 0.3895(3) 0.7218(2) 0.6260(3) 0.0276(10) Uani 1 1 d .
C19 C 0.4664(3) 0.6601(2) 0.6554(3) 0.0274(10) Uani 1 1 d .
C11 C 0.0650(3) 0.7430(3) 0.6116(3) 0.0354(11) Uani 1 1 d .
H11 H 0.0470 0.7863 0.5684 0.042 Uiso 1 1 calc R
C14 C 0.3794(3) 0.7725(2) 0.6935(3) 0.0259(9) Uani 1 1 d .
C18 C 0.6202(3) 0.5925(3) 0.7937(3) 0.0296(10) Uani 1 1 d .
C15 C 0.4393(3) 0.7578(3) 0.7848(3) 0.0310(10) Uani 1 1 d .
H15 H 0.4297 0.7881 0.8286 0.037 Uiso 1 1 calc R
C7 C 0.0639(3) 0.6800(2) 0.7474(3) 0.0238(9) Uani 1 1 d .
C4 C -0.0326(3) 0.7463(3) 0.8124(3) 0.0304(10) Uani 1 1 d .
H4 H -0.0548 0.7476 0.8564 0.036 Uiso 1 1 calc R
C2 C -0.0315(3) 0.8098(2) 0.6805(3) 0.0247(9) Uani 1 1 d .
C27 C 0.2145(4) 1.0863(3) 0.8523(3) 0.0475(13) Uani 1 1 d .
H27 H 0.2546 1.1263 0.8446 0.057 Uiso 1 1 calc R
C17 C 0.5308(3) 0.6504(2) 0.7519(3) 0.0268(10) Uani 1 1 d .
C20 C 0.4743(4) 0.6103(3) 0.5874(3) 0.0413(12) Uani 1 1 d .
H20 H 0.5241 0.5702 0.6052 0.050 Uiso 1 1 calc R
C3 C -0.0654(3) 0.8086(3) 0.7440(3) 0.0314(11) Uani 1 1 d .
H3 H -0.1104 0.8492 0.7419 0.038 Uiso 1 1 calc R
N3 N 0.1779(4) 1.0956(3) 0.9104(3) 0.0625(14) Uani 1 1 d .
C23 C 0.3243(3) 0.7297(3) 0.5306(3) 0.0362(11) Uani 1 1 d .
H23 H 0.2737 0.7693 0.5109 0.043 Uiso 1 1 calc R
C12 C 0.0333(3) 0.7459(2) 0.6802(3) 0.0235(9) Uani 1 1 d .
C1 C -0.0658(3) 0.8804(2) 0.6095(3) 0.0265(10) Uani 1 1 d .
C16 C 0.5145(3) 0.6979(3) 0.8129(3) 0.0320(10) Uani 1 1 d .
H16 H 0.5551 0.6901 0.8754 0.038 Uiso 1 1 calc R
C5 C 0.0306(3) 0.6838(2) 0.8165(3) 0.0221(9) Uani 1 1 d .
C8 C 0.1208(3) 0.6131(3) 0.7399(3) 0.0417(12) Uani 1 1 d .
H8 H 0.1393 0.5686 0.7816 0.050 Uiso 1 1 calc R
C21 C 0.4100(4) 0.6200(3) 0.4959(3) 0.0512(14) Uani 1 1 d .
H21 H 0.4166 0.5863 0.4526 0.061 Uiso 1 1 calc R
C9 C 0.1493(4) 0.6124(3) 0.6722(3) 0.0516(14) Uani 1 1 d .
H9 H 0.1876 0.5681 0.6691 0.062 Uiso 1 1 calc R
C22 C 0.3346(4) 0.6803(3) 0.4673(3) 0.0469(13) Uani 1 1 d .
H22 H 0.2914 0.6868 0.4052 0.056 Uiso 1 1 calc R
C10 C 0.1214(4) 0.6779(3) 0.6080(3) 0.0472(13) Uani 1 1 d .
H10 H 0.1414 0.6771 0.5624 0.057 Uiso 1 1 calc R
C28 C 0.1919(5) 1.1671(4) 0.9720(4) 0.086(2) Uani 1 1 d U
H28A H 0.1285 1.1835 0.9669 0.103 Uiso 1 1 calc R
H28B H 0.2175 1.2149 0.9526 0.103 Uiso 1 1 calc R
C25 C 0.1301(4) 0.9751(4) 0.8362(4) 0.0713(19) Uani 1 1 d .
H25 H 0.0993 0.9230 0.8163 0.086 Uiso 1 1 calc R
C26 C 0.1245(4) 1.0258(5) 0.9009(4) 0.078(2) Uani 1 1 d .
H26 H 0.0894 1.0138 0.9331 0.094 Uiso 1 1 calc R
H1 H 0.143(5) 1.0727(11) 0.592(5) 0.118 Uiso 1 1 d D
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
C38 N1 C37 105.1(3) . .
C38 N1 Zn3 124.8(3) . 1_556
C37 N1 Zn3 129.9(3) . 1_556
N1 C38 N2 112.0(4) . .
C36 C37 N1 109.6(4) . .
C6 O3 Zn3 137.4(3) . 4_576
C6 O4 Zn1 124.6(2) . 2_546
O3 C6 O4 125.4(4) . .
O3 C6 C5 117.5(3) . .
O4 C6 C5 117.0(4) . .
C18 O8 Zn2 123.0(3) . 2_646
C18 O7 Zn3 139.0(3) . 2_646
C37 C36 N2 107.1(4) . .
C38 N2 C36 106.1(4) . .
C38 N2 C35 126.5(4) . .
C36 N2 C35 127.1(4) . .
N2 C35 C32 110.4(4) . .
C33 C32 C31 118.2(5) . .
C33 C32 C35 120.7(5) . .
C31 C32 C35 121.1(5) . .
C32 C33 C34 121.1(5) . .
C29 C34 C33 120.6(5) . .
C32 C31 C30 121.4(5) . .
C31 C30 C29 120.0(5) . .
C34 C29 C30 118.7(5) . .
C34 C29 C28 117.6(5) . .
C30 C29 C28 123.7(5) . .
C1 O2 Zn3 125.2(3) . 3_576
O9 Zn1 O9 180.000(1) 3_576 .
O9 Zn1 O1 87.20(10) 3_576 3_576
O9 Zn1 O1 92.80(11) . 3_576
O9 Zn1 O1 92.80(11) 3_576 .
O9 Zn1 O1 87.20(10) . .
O1 Zn1 O1 180.000(1) 3_576 .
O9 Zn1 O4 80.70(10) 3_576 4_575
O9 Zn1 O4 99.30(10) . 4_575
O1 Zn1 O4 91.08(11) 3_576 4_575
O1 Zn1 O4 88.92(11) . 4_575
O9 Zn1 O4 99.30(10) 3_576 2_556
O9 Zn1 O4 80.70(10) . 2_556
O1 Zn1 O4 88.92(11) 3_576 2_556
O1 Zn1 O4 91.08(11) . 2_556
O4 Zn1 O4 180.00(13) 4_575 2_556
O5 Zn2 O9 115.70(12) . .
O5 Zn2 N4 112.87(14) . .
O9 Zn2 N4 119.51(13) . .
O5 Zn2 O8 107.58(14) . 2_656
O9 Zn2 O8 102.31(12) . 2_656
N4 Zn2 O8 95.12(14) . 2_656
O3 Zn3 N1 87.75(12) 4_575 1_554
O3 Zn3 O9 101.44(11) 4_575 .
N1 Zn3 O9 170.51(12) 1_554 .
O3 Zn3 O2 96.50(13) 4_575 3_576
N1 Zn3 O2 90.36(12) 1_554 3_576
O9 Zn3 O2 86.30(11) . 3_576
O3 Zn3 O6 85.26(13) 4_575 .
N1 Zn3 O6 92.50(12) 1_554 .
O9 Zn3 O6 90.63(11) . .
O2 Zn3 O6 176.70(11) 3_576 .
O3 Zn3 O7 168.31(13) 4_575 2_656
N1 Zn3 O7 84.25(12) 1_554 2_656
O9 Zn3 O7 87.00(11) . 2_656
O2 Zn3 O7 92.07(13) 3_576 2_656
O6 Zn3 O7 86.59(14) . 2_656
Zn2 O9 Zn3 107.79(12) . .
Zn2 O9 Zn1 128.62(13) . .
Zn3 O9 Zn1 111.02(12) . .
C1 O1 Zn1 131.8(3) . .
C13 O5 Zn2 114.5(3) . .
C13 O6 Zn3 146.1(3) . .
O6 C13 O5 125.4(4) . .
O6 C13 C14 118.5(4) . .
O5 C13 C14 115.9(4) . .
C27 N4 C25 105.1(4) . .
C27 N4 Zn2 122.4(3) . .
C25 N4 Zn2 132.5(4) . .
C23 C24 C19 118.7(4) . .
C23 C24 C14 122.2(4) . .
C19 C24 C14 119.1(4) . .
C20 C19 C24 118.0(4) . .
C20 C19 C17 123.1(4) . .
C24 C19 C17 118.8(4) . .
C10 C11 C12 121.0(4) . .
C15 C14 C24 119.8(4) . .
C15 C14 C13 116.8(4) . .
C24 C14 C13 123.0(4) . .
O7 C18 O8 124.9(4) . .
O7 C18 C17 116.0(4) . .
O8 C18 C17 119.1(4) . .
C14 C15 C16 120.6(4) . .
C8 C7 C12 118.2(4) . .
C8 C7 C5 123.8(4) . .
C12 C7 C5 118.0(3) . .
C5 C4 C3 122.2(4) . .
C3 C2 C12 120.5(4) . .
C3 C2 C1 118.6(4) . .
C12 C2 C1 121.0(3) . .
N3 C27 N4 113.1(5) . .
C16 C17 C19 119.1(4) . .
C16 C17 C18 115.6(4) . .
C19 C17 C18 125.2(4) . .
C21 C20 C19 121.5(4) . .
C2 C3 C4 120.1(4) . .
C27 N3 C26 105.4(5) . .
C27 N3 C28 127.6(6) . .
C26 N3 C28 127.0(6) . .
C22 C23 C24 121.3(4) . .
C2 C12 C11 121.5(4) . .
C2 C12 C7 119.7(3) . .
C11 C12 C7 118.7(4) . .
O1 C1 O2 126.9(4) . .
O1 C1 C2 116.8(4) . .
O2 C1 C2 116.3(4) . .
C17 C16 C15 122.3(4) . .
C4 C5 C7 119.5(3) . .
C4 C5 C6 117.7(4) . .
C7 C5 C6 122.8(3) . .
C9 C8 C7 121.2(4) . .
C20 C21 C22 120.3(4) . .
C8 C9 C10 120.5(4) . .
C23 C22 C21 120.1(4) . .
C11 C10 C9 120.4(4) . .
N3 C28 C29 113.0(5) . .
N4 C25 C26 107.8(6) . .
N3 C26 C25 108.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C38 1.312(5) .
N1 C37 1.359(5) .
N1 Zn3 2.048(3) 1_556
C38 N2 1.341(5) .
C37 C36 1.343(6) .
O3 C6 1.245(5) .
O3 Zn3 2.040(3) 4_576
O4 C6 1.262(5) .
O4 Zn1 2.123(3) 2_546
C6 C5 1.518(5) .
O8 C18 1.263(5) .
O8 Zn2 2.017(3) 2_646
O7 C18 1.242(5) .
O7 Zn3 2.196(3) 2_646
C36 N2 1.353(6) .
N2 C35 1.459(5) .
C35 C32 1.509(6) .
C32 C33 1.370(7) .
C32 C31 1.373(6) .
C33 C34 1.374(7) .
C34 C29 1.372(6) .
C31 C30 1.373(7) .
C30 C29 1.382(7) .
C29 C28 1.508(7) .
O2 C1 1.260(5) .
O2 Zn3 2.139(3) 3_576
Zn1 O9 2.086(3) 3_576
Zn1 O9 2.086(3) .
Zn1 O1 2.098(3) 3_576
Zn1 O1 2.098(3) .
Zn1 O4 2.123(3) 4_575
Zn1 O4 2.123(3) 2_556
Zn2 O5 1.935(3) .
Zn2 O9 1.937(3) .
Zn2 N4 1.993(4) .
Zn2 O8 2.017(3) 2_656
Zn3 O3 2.040(3) 4_575
Zn3 N1 2.048(3) 1_554
Zn3 O9 2.048(3) .
Zn3 O2 2.139(3) 3_576
Zn3 O6 2.176(3) .
Zn3 O7 2.196(3) 2_656
O1 C1 1.257(5) .
O5 C13 1.277(5) .
O6 C13 1.227(5) .
C13 C14 1.517(5) .
N4 C27 1.323(6) .
N4 C25 1.352(6) .
C24 C23 1.420(6) .
C24 C19 1.431(6) .
C24 C14 1.433(6) .
C19 C20 1.415(6) .
C19 C17 1.437(6) .
C11 C10 1.361(6) .
C11 C12 1.419(5) .
C14 C15 1.368(6) .
C18 C17 1.520(5) .
C15 C16 1.394(6) .
C7 C8 1.413(6) .
C7 C12 1.429(5) .
C7 C5 1.444(5) .
C4 C5 1.363(5) .
C4 C3 1.400(5) .
C2 C3 1.364(5) .
C2 C12 1.418(5) .
C2 C1 1.520(5) .
C27 N3 1.319(6) .
C17 C16 1.363(6) .
C20 C21 1.371(6) .
N3 C26 1.338(8) .
N3 C28 1.465(7) .
C23 C22 1.366(6) .
C8 C9 1.368(6) .
C21 C22 1.400(7) .
C9 C10 1.397(6) .
C25 C26 1.364(8) .
