#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:59:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180459 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/28/7212899.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_7212899
loop_
_publ_author_name
'Qin, Jie'
'Qin, Chao'
'Wang, Cui-Xia'
'Li, Huan'
'Cui, Ling'
'Li, Ting-Ting'
'Wang, Xin-Long'
_publ_section_title
;
 A lacuna in reticular chemistry: an unprecedented binodal
 (6,10)-connected network based on two distinct zinc clusters
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4071
_journal_paper_doi               10.1039/c0ce00582g
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C44 H56 N18 O30 Zn7'
_chemical_formula_weight         1774.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.50(3)
_cell_angle_beta                 99.07(3)
_cell_angle_gamma                112.41(3)
_cell_formula_units_Z            1
_cell_length_a                   9.781(2)
_cell_length_b                   11.905(2)
_cell_length_c                   15.220(3)
_cell_measurement_reflns_used    12474
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.19
_cell_volume                     1588.5(7)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12474
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    2.700
_exptl_absorpt_correction_T_max  0.7202
_exptl_absorpt_correction_T_min  0.6702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         5549
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0655P)²+3.0476P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                4781
_reflns_number_total             5549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00582g.txt
_cod_data_source_block           www
_cod_original_cell_volume        1588.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7212899
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.5000 0.5000 0.01282(15) Uani 1 2 d S . .
Zn2 Zn -0.01127(5) 0.57029(5) 0.29485(3) 0.02077(14) Uani 1 1 d . . .
Zn3 Zn 0.10931(5) 0.31173(5) 0.32978(3) 0.02221(14) Uani 1 1 d . . .
Zn4 Zn 0.43913(5) 0.60484(5) 0.07046(3) 0.02049(14) Uani 1 1 d . . .
C1 C -0.3396(5) 0.1593(4) 0.1939(3) 0.0242(9) Uani 1 1 d . . .
C2 C -0.3790(5) 0.0345(4) 0.1629(3) 0.0268(10) Uani 1 1 d . . .
H2A H -0.3080 0.0013 0.1764 0.032 Uiso 1 1 calc R . .
C3 C -0.5220(5) -0.0409(4) 0.1123(3) 0.0318(10) Uani 1 1 d . . .
C4 C -0.6262(6) 0.0103(5) 0.0913(4) 0.0430(13) Uani 1 1 d . . .
H4A H -0.7231 -0.0396 0.0575 0.052 Uiso 1 1 calc R . .
C5 C -0.5869(6) 0.1342(5) 0.1202(4) 0.0457(14) Uani 1 1 d . . .
H5A H -0.6563 0.1682 0.1042 0.055 Uiso 1 1 calc R . .
C6 C -0.4449(5) 0.2087(5) 0.1731(3) 0.0320(10) Uani 1 1 d . . .
H6A H -0.4203 0.2919 0.1945 0.038 Uiso 1 1 calc R . .
C7 C -0.1871(5) 0.2390(4) 0.2521(3) 0.0265(10) Uani 1 1 d . . .
C8 C -0.5645(6) -0.1754(5) 0.0834(3) 0.0364(12) Uani 1 1 d . . .
C9 C 0.3999(5) 0.1315(4) 0.3719(3) 0.0232(9) Uani 1 1 d . . .
C10 C 0.2989(5) 0.0090(4) 0.3546(3) 0.0248(9) Uani 1 1 d . . .
H10A H 0.1960 -0.0114 0.3349 0.030 Uiso 1 1 calc R . .
C11 C 0.3485(5) -0.0843(4) 0.3659(3) 0.0256(9) Uani 1 1 d . . .
C12 C 0.5042(5) -0.0526(5) 0.3922(3) 0.0318(11) Uani 1 1 d . . .
H12A H 0.5395 -0.1139 0.3997 0.038 Uiso 1 1 calc R . .
C13 C 0.6050(5) 0.0688(5) 0.4070(4) 0.0337(11) Uani 1 1 d . . .
H13A H 0.7085 0.0889 0.4228 0.040 Uiso 1 1 calc R . .
C14 C 0.5542(5) 0.1621(4) 0.3985(3) 0.0272(10) Uani 1 1 d . . .
H14A H 0.6230 0.2444 0.4105 0.033 Uiso 1 1 calc R . .
C15 C 0.3425(5) 0.2305(4) 0.3631(3) 0.0248(9) Uani 1 1 d . . .
C16 C 0.2384(5) -0.2151(4) 0.3541(3) 0.0260(9) Uani 1 1 d . . .
C17 C 0.1931(5) 0.5721(4) 0.1712(3) 0.0273(10) Uani 1 1 d . . .
H17A H 0.1725 0.6331 0.1462 0.033 Uiso 1 1 calc R . .
C18 C 0.2881(5) 0.4478(5) 0.2024(3) 0.0283(10) Uani 1 1 d . . .
H18A H 0.3480 0.4030 0.2037 0.034 Uiso 1 1 calc R . .
C19 C 0.0315(5) 0.3701(4) 0.5077(3) 0.0232(9) Uani 1 1 d . . .
H19A H -0.0714 0.3216 0.4860 0.028 Uiso 1 1 calc R . .
C20 C 0.2392(5) 0.4866(4) 0.5922(3) 0.0245(9) Uani 1 1 d . . .
H20A H 0.3126 0.5381 0.6426 0.029 Uiso 1 1 calc R . .
C21 C -0.2884(5) 0.5959(5) 0.1877(3) 0.0316(11) Uani 1 1 d . . .
H21A H -0.2915 0.6504 0.2354 0.038 Uiso 1 1 calc R . .
C22 C -0.2236(5) 0.4766(4) 0.1096(3) 0.0258(10) Uani 1 1 d . . .
H22A H -0.1715 0.4305 0.0911 0.031 Uiso 1 1 calc R . .
N1 N 0.1834(4) 0.4321(3) 0.2497(2) 0.0232(8) Uani 1 1 d . . .
N2 N 0.1212(4) 0.5139(3) 0.2285(2) 0.0228(8) Uani 1 1 d . . .
N3 N 0.2999(4) 0.5347(4) 0.1521(2) 0.0246(8) Uani 1 1 d . . .
N4 N 0.1332(4) 0.3853(3) 0.4582(2) 0.0238(8) Uani 1 1 d . . .
N5 N 0.2701(4) 0.4609(3) 0.5143(2) 0.0230(8) Uani 1 1 d . . .
N6 N 0.0925(4) 0.4323(3) 0.5928(2) 0.0222(7) Uani 1 1 d . . .
N7 N -0.1839(4) 0.5492(4) 0.1911(2) 0.0247(8) Uani 1 1 d . . .
N8 N -0.3450(4) 0.4777(3) 0.0582(2) 0.0222(8) Uani 1 1 d . . .
N9 N -0.3879(4) 0.5557(4) 0.1084(2) 0.0271(8) Uani 1 1 d . . .
O1 O -0.1538(4) 0.3488(3) 0.2818(2) 0.0361(8) Uani 1 1 d . . .
O2 O -0.0940(4) 0.1880(3) 0.2696(2) 0.0356(8) Uani 1 1 d . . .
O3 O -0.4631(4) -0.2159(3) 0.1057(3) 0.0440(9) Uani 1 1 d . . .
O4 O -0.6941(4) -0.2454(3) 0.0426(3) 0.0463(9) Uani 1 1 d . . .
O5 O 0.4291(3) 0.3418(3) 0.3852(2) 0.0316(7) Uani 1 1 d . . .
O6 O 0.2015(4) 0.1930(3) 0.3313(3) 0.0370(8) Uani 1 1 d . . .
O7 O 0.1070(3) -0.2449(3) 0.3042(2) 0.0316(7) Uani 1 1 d . . .
O8 O 0.2724(4) -0.2904(3) 0.3921(2) 0.0360(8) Uani 1 1 d . . .
O1W O 0.5046(4) 0.3795(3) 0.5926(2) 0.0354(8) Uani 1 1 d . . .
H1 H 0.5775 0.3598 0.5891 0.035 Uiso 1 1 d R . .
H2 H 0.4287 0.3147 0.5916 0.035 Uiso 1 1 d R . .
OW1 O 0.9984(8) 0.7293(9) 0.9881(7) 0.158(4) Uani 1 1 d . . .
OW2 O 0.9696(11) 0.9066(11) 0.8850(7) 0.161(4) Uani 1 1 d . . .
OW3 O 0.9957(11) 0.8475(11) 0.1537(9) 0.183(5) Uani 1 1 d . . .
OW4 O 0.7687(6) 0.8112(6) 0.4113(6) 0.100(2) Uani 1 1 d . . .
OW5 O 0.8992(13) 0.9774(11) 0.3420(10) 0.081(3) Uani 0.50 1 d PU A 1
OW6 O 0.9654(14) 1.0030(13) 0.4412(9) 0.095(4) Uani 0.50 1 d P . 1
OW5' O 0.828(3) 0.9009(16) 0.3051(12) 0.196(12) Uani 0.50 1 d P B 2
OW6' O 0.8739(18) 0.8937(18) 0.4637(12) 0.119(5) Uani 0.50 1 d P B 2
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
O1W Zn1 O1W 180.000(1) 2_666 .
O1W Zn1 N5 93.21(13) 2_666 .
O1W Zn1 N5 86.79(13) . .
O1W Zn1 N5 86.79(13) 2_666 2_666
O1W Zn1 N5 93.21(13) . 2_666
N5 Zn1 N5 180.000(1) . 2_666
O1W Zn1 O5 89.47(13) 2_666 2_666
O1W Zn1 O5 90.53(13) . 2_666
N5 Zn1 O5 86.17(13) . 2_666
N5 Zn1 O5 93.83(13) 2_666 2_666
O1W Zn1 O5 90.53(13) 2_666 .
O1W Zn1 O5 89.47(13) . .
N5 Zn1 O5 93.83(13) . .
N5 Zn1 O5 86.17(13) 2_666 .
O5 Zn1 O5 180.0 2_666 .
N6 Zn2 N2 144.40(14) 2_566 .
N6 Zn2 O7 101.11(15) 2_566 1_565
N2 Zn2 O7 96.96(14) . 1_565
N6 Zn2 N7 106.39(14) 2_566 .
N2 Zn2 N7 101.62(15) . .
O7 Zn2 N7 96.64(15) 1_565 .
N6 Zn2 O1 79.39(14) 2_566 .
N2 Zn2 O1 82.82(13) . .
O7 Zn2 O1 179.35(13) 1_565 .
N7 Zn2 O1 82.82(14) . .
O6 Zn3 O2 94.54(14) . .
O6 Zn3 N1 113.33(15) . .
O2 Zn3 N1 109.05(15) . .
O6 Zn3 N4 106.92(16) . .
O2 Zn3 N4 115.63(16) . .
N1 Zn3 N4 115.54(16) . .
O3 Zn4 N8 121.39(16) 1_665 2_565
O3 Zn4 N3 109.98(16) 1_665 .
N8 Zn4 N3 111.39(15) 2_565 .
O3 Zn4 N9 102.03(17) 1_665 1_655
N8 Zn4 N9 106.59(15) 2_565 1_655
N3 Zn4 N9 103.42(15) . 1_655
C2 C1 C6 119.4(4) . .
C2 C1 C7 120.6(4) . .
C6 C1 C7 119.9(4) . .
C3 C2 C1 120.9(4) . .
C3 C2 H2A 119.5 . .
C1 C2 H2A 119.5 . .
C2 C3 C4 118.9(5) . .
C2 C3 C8 120.2(4) . .
C4 C3 C8 120.8(4) . .
C5 C4 C3 120.4(5) . .
C5 C4 H4A 119.8 . .
C3 C4 H4A 119.8 . .
C4 C5 C6 120.5(5) . .
C4 C5 H5A 119.8 . .
C6 C5 H5A 119.8 . .
C5 C6 C1 119.8(5) . .
C5 C6 H6A 120.1 . .
C1 C6 H6A 120.1 . .
O1 C7 O2 122.2(4) . .
O1 C7 C1 120.6(4) . .
O2 C7 C1 117.2(4) . .
O4 C8 O3 121.5(5) . .
O4 C8 C3 121.2(5) . .
O3 C8 C3 117.3(4) . .
C10 C9 C14 119.7(4) . .
C10 C9 C15 119.9(4) . .
C14 C9 C15 120.4(4) . .
C9 C10 C11 121.1(4) . .
C9 C10 H10A 119.5 . .
C11 C10 H10A 119.5 . .
C10 C11 C12 118.7(4) . .
C10 C11 C16 120.9(4) . .
C12 C11 C16 120.4(4) . .
C13 C12 C11 120.2(4) . .
C13 C12 H12A 119.9 . .
C11 C12 H12A 119.9 . .
C12 C13 C14 120.7(4) . .
C12 C13 H13A 119.7 . .
C14 C13 H13A 119.7 . .
C9 C14 C13 119.5(4) . .
C9 C14 H14A 120.2 . .
C13 C14 H14A 120.2 . .
O5 C15 O6 122.9(4) . .
O5 C15 C9 121.4(4) . .
O6 C15 C9 115.7(4) . .
O8 C16 O7 122.0(4) . .
O8 C16 C11 121.2(4) . .
O7 C16 C11 116.7(4) . .
N2 C17 N3 112.9(4) . .
N2 C17 H17A 123.5 . .
N3 C17 H17A 123.5 . .
N1 C18 N3 113.1(4) . .
N1 C18 H18A 123.4 . .
N3 C18 H18A 123.4 . .
N4 C19 N6 112.4(4) . .
N4 C19 H19A 123.8 . .
N6 C19 H19A 123.8 . .
N5 C20 N6 113.7(4) . .
N5 C20 H20A 123.2 . .
N6 C20 H20A 123.2 . .
N7 C21 N9 112.6(4) . .
N7 C21 H21A 123.7 . .
N9 C21 H21A 123.7 . .
N8 C22 N7 112.5(4) . .
N8 C22 H22A 123.7 . .
N7 C22 H22A 123.7 . .
C18 N1 N2 105.4(3) . .
C18 N1 Zn3 130.7(3) . .
N2 N1 Zn3 123.8(3) . .
C17 N2 N1 106.3(3) . .
C17 N2 Zn2 124.0(3) . .
N1 N2 Zn2 127.8(3) . .
C18 N3 C17 102.3(3) . .
C18 N3 Zn4 132.4(3) . .
C17 N3 Zn4 125.2(3) . .
C19 N4 N5 106.2(3) . .
C19 N4 Zn3 130.0(3) . .
N5 N4 Zn3 123.8(3) . .
C20 N5 N4 105.3(3) . .
C20 N5 Zn1 121.9(3) . .
N4 N5 Zn1 131.1(3) . .
C19 N6 C20 102.4(4) . .
C19 N6 Zn2 132.9(3) . 2_566
C20 N6 Zn2 123.8(3) . 2_566
C21 N7 C22 103.1(4) . .
C21 N7 Zn2 130.3(3) . .
C22 N7 Zn2 126.5(3) . .
C22 N8 N9 106.4(3) . .
C22 N8 Zn4 127.8(3) . 2_565
N9 N8 Zn4 125.6(3) . 2_565
C21 N9 N8 105.4(3) . .
C21 N9 Zn4 126.8(3) . 1_455
N8 N9 Zn4 127.7(3) . 1_455
C7 O1 Zn2 154.1(3) . .
C7 O2 Zn3 111.2(3) . .
C8 O3 Zn4 106.8(3) . 1_445
C15 O5 Zn1 139.7(3) . .
C15 O6 Zn3 119.5(3) . .
C16 O7 Zn2 107.4(3) . 1_545
Zn1 O1W H1 108.2 . .
Zn1 O1W H2 121.9 . .
H1 O1W H2 107.8 . .
OW6' OW4 OW5' 90.2(9) . .
OW5 OW6 OW6 167.2(15) . 2_776
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1W 2.130(3) 2_666
Zn1 O1W 2.130(3) .
Zn1 N5 2.168(3) .
Zn1 N5 2.168(3) 2_666
Zn1 O5 2.226(3) 2_666
Zn1 O5 2.226(3) .
Zn2 N6 1.994(4) 2_566
Zn2 N2 2.018(3) .
Zn2 O7 2.034(3) 1_565
Zn2 N7 2.039(3) .
Zn2 O1 2.435(4) .
Zn3 O6 1.946(3) .
Zn3 O2 1.962(3) .
Zn3 N1 1.986(4) .
Zn3 N4 1.988(4) .
Zn4 O3 1.944(4) 1_665
Zn4 N8 1.989(4) 2_565
Zn4 N3 1.999(4) .
Zn4 N9 2.014(3) 1_655
C1 C2 1.388(6) .
C1 C6 1.382(6) .
C1 C7 1.491(6) .
C2 C3 1.379(7) .
C2 H2A 0.9300 .
C3 C4 1.388(7) .
C3 C8 1.485(7) .
C4 C5 1.373(8) .
C4 H4A 0.9300 .
C5 C6 1.382(7) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
C7 O1 1.231(6) .
C7 O2 1.284(5) .
C8 O4 1.232(6) .
C8 O3 1.276(6) .
C9 C10 1.380(6) .
C9 C14 1.389(6) .
C9 C15 1.496(6) .
C10 C11 1.388(6) .
C10 H10A 0.9300 .
C11 C12 1.399(6) .
C11 C16 1.488(6) .
C12 C13 1.372(7) .
C12 H12A 0.9300 .
C13 C14 1.389(7) .
C13 H13A 0.9300 .
C14 H14A 0.9300 .
C15 O5 1.242(5) .
C15 O6 1.267(5) .
C16 O8 1.237(5) .
C16 O7 1.280(5) .
C17 N2 1.302(6) .
C17 N3 1.339(5) .
C17 H17A 0.9300 .
C18 N1 1.311(6) .
C18 N3 1.336(6) .
C18 H18A 0.9300 .
C19 N4 1.312(5) .
C19 N6 1.336(5) .
C19 H19A 0.9300 .
C20 N5 1.301(6) .
C20 N6 1.333(6) .
C20 H20A 0.9300 .
C21 N7 1.334(6) .
C21 N9 1.333(6) .
C21 H21A 0.9300 .
C22 N8 1.320(5) .
C22 N7 1.337(6) .
C22 H22A 0.9300 .
N1 N2 1.372(5) .
N4 N5 1.371(5) .
N6 Zn2 1.994(4) 2_566
N8 N9 1.364(5) .
N8 Zn4 1.989(4) 2_565
N9 Zn4 2.014(3) 1_455
O3 Zn4 1.944(4) 1_445
O7 Zn2 2.034(3) 1_545
O1W H1 0.8378 .
O1W H2 0.8386 .
OW4 OW6' 1.206(19) .
OW4 OW5' 2.07(3) .
OW5 OW6 1.493(17) .
OW6 OW6 1.83(3) 2_776
