#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/16/7001648.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_7001648
loop_
_publ_author_name
'Liu, Jian-Qiang'
'Zhang, Ya-Nan'
'Wang, Yao-Yu'
'Jin, Jun-Cheng'
'Lermontova, Elmira Kh.'
'Shi, Qi-Zhen'
_publ_section_title
;
 Interplay of coordinative and supramolecular interactions in formation
 of a series of metal--organic complexes bearing diverse
 dimensionalities
;
_journal_issue                   27
_journal_name_full               'Dalton Transactions'
_journal_page_first              5365
_journal_page_last               5378
_journal_paper_doi               10.1039/b822083b
_journal_year                    2009
_chemical_formula_moiety         'C29H16N4O8Zn2, 2.5(H2O)'
_chemical_formula_sum            'C29 H21 N4 O10.5 Zn2'
_chemical_formula_weight         724.24
_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                102.897(5)
_cell_angle_beta                 99.497(4)
_cell_angle_gamma                105.805(4)
_cell_formula_units_Z            2
_cell_length_a                   9.079(2)
_cell_length_b                   12.415(3)
_cell_length_c                   13.982(3)
_cell_measurement_reflns_used    5060
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      1.54
_cell_volume                     1434.7(6)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX SMART II'
_diffrn_measurement_method       ω
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.1557
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7322
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  0.7563
_exptl_absorpt_correction_T_min  0.6232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5060
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                2325
_reflns_number_total             5060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b822083b.txt
_cod_data_source_block           compound15
_cod_original_cell_volume        1434.7(5)
_cod_original_formula_sum        'C29 H21 N4 O10.50 Zn2'
_cod_database_code               7001648
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
C28 C 1.6188(7) 0.9553(7) 1.0271(5) 0.0421(19) Uani 1 1 d . . .
H28 H 1.6989 0.9251 1.0452 0.050 Uiso 1 1 calc R . .
O3W O 0.8944(18) 0.6202(11) 0.3209(9) 0.152(6) Uani 0.50 1 d PD . .
H5W H 0.8858 0.6521 0.3709 0.227 Uiso 0.50 1 d PRD . .
H6W H 0.9717 0.6450 0.2931 0.227 Uiso 0.50 1 d PRD . .
O2 O 0.9282(5) 1.1007(4) 0.5421(3) 0.0442(12) Uani 1 1 d . . .
C29 C 1.4680(7) 0.8801(6) 0.9800(5) 0.0412(18) Uani 1 1 d . . .
H29 H 1.4472 0.7999 0.9668 0.049 Uiso 1 1 calc R . .
C25 C 0.3478(8) 0.4569(7) 0.9420(5) 0.060(2) Uani 1 1 d . . .
H25 H 0.2453 0.4278 0.9020 0.072 Uiso 1 1 calc R . .
C21 C 0.4128(7) 0.4884(6) 0.4041(5) 0.0457(19) Uani 1 1 d . . .
H21 H 0.3557 0.4806 0.3399 0.055 Uiso 1 1 calc R . .
C17 C 0.3867(7) 0.8917(6) 0.4751(4) 0.0375(17) Uani 1 1 d . . .
H17 H 0.3108 0.8186 0.4580 0.045 Uiso 1 1 calc R . .
C24 C 0.4626(9) 0.5392(7) 0.9171(5) 0.059(2) Uani 1 1 d . . .
H24 H 0.4359 0.5654 0.8614 0.070 Uiso 1 1 calc R . .
C16 C 0.5455(7) 0.9039(7) 0.5090(5) 0.0437(19) Uani 1 1 d . . .
H16 H 0.5752 0.8393 0.5153 0.052 Uiso 1 1 calc R . .
N1 N 0.2062(6) 0.8098(5) 0.6496(4) 0.0406(14) Uani 1 1 d . . .
N2 N 0.2342(6) 1.0343(6) 0.6857(4) 0.0423(15) Uani 1 1 d . . .
C13 C 0.3674(7) 1.0083(7) 0.7175(4) 0.0411(19) Uani 1 1 d . . .
C5 C 0.3500(7) 0.8839(6) 0.6989(4) 0.0351(17) Uani 1 1 d . . .
C1 C 0.1860(8) 0.6972(7) 0.6327(5) 0.052(2) Uani 1 1 d . . .
H1 H 0.0866 0.6449 0.5984 0.062 Uiso 1 1 calc R . .
C2 C 0.3040(8) 0.6522(7) 0.6628(5) 0.055(2) Uani 1 1 d . . .
H2 H 0.2835 0.5720 0.6500 0.066 Uiso 1 1 calc R . .
Zn1 Zn 1.04044(8) 0.88710(7) 0.59580(6) 0.0377(3) Uani 1 1 d . . .
Zn2 Zn 0.86185(8) 0.79632(8) 0.82479(6) 0.0449(3) Uani 1 1 d . . .
O7 O 1.0792(5) 0.8906(5) 0.8815(3) 0.0622(15) Uani 1 1 d . . .
C6 C 0.6256(7) 0.9375(7) 0.7794(4) 0.0346(17) Uani 1 1 d . . .
O1 O 0.8630(5) 0.9557(4) 0.6127(3) 0.0496(13) Uani 1 1 d . . .
N3 N 0.7732(6) 0.9274(5) 0.8192(4) 0.0361(14) Uani 1 1 d . . .
O3 O 0.8644(5) 0.7305(4) 0.5271(3) 0.0549(14) Uani 1 1 d . . .
N4 N 0.7980(6) 1.1167(6) 0.8429(4) 0.0483(16) Uani 1 1 d . . .
H4 H 0.8423 1.1912 0.8609 0.058 Uiso 1 1 calc R . .
O4 O 0.8488(5) 0.7223(4) 0.6818(3) 0.0546(14) Uani 1 1 d . . .
C18 C 0.7960(7) 0.6884(6) 0.5871(6) 0.0426(18) Uani 1 1 d . . .
O5 O 0.7166(5) 0.6734(5) 0.8579(4) 0.0655(16) Uani 1 1 d . . .
O8 O 1.1568(6) 0.7365(6) 0.8822(4) 0.0739(17) Uani 1 1 d . . .
C7 C 0.6393(7) 1.0544(7) 0.7944(5) 0.0381(17) Uani 1 1 d . . .
C8 C 0.8653(8) 1.0368(7) 0.8552(5) 0.0470(19) Uani 1 1 d . . .
H8 H 0.9712 1.0568 0.8872 0.056 Uiso 1 1 calc R . .
C3 C 0.4501(8) 0.7276(7) 0.7116(5) 0.052(2) Uani 1 1 d . . .
H3 H 0.5313 0.6993 0.7322 0.062 Uiso 1 1 calc R . .
C27 C 1.3477(7) 0.9246(7) 0.9522(4) 0.0381(18) Uani 1 1 d . . .
C9 C 0.5108(8) 1.0944(7) 0.7655(5) 0.0384(17) Uani 1 1 d . . .
C4 C 0.4786(7) 0.8483(7) 0.7309(5) 0.0387(18) Uani 1 1 d . . .
C20 C 0.5540(7) 0.5779(6) 0.4469(5) 0.0454(19) Uani 1 1 d . . .
H20 H 0.5903 0.6309 0.4117 0.054 Uiso 1 1 calc R . .
C26 C 1.1819(8) 0.8426(8) 0.9017(5) 0.049(2) Uani 1 1 d . . .
C19 C 0.6436(7) 0.5898(6) 0.5432(5) 0.0383(17) Uani 1 1 d . . .
C12 C 0.2464(8) 1.1463(8) 0.7036(5) 0.056(2) Uani 1 1 d . . .
H12 H 0.1562 1.1653 0.6831 0.067 Uiso 1 1 calc R . .
C14 C 0.8292(7) 1.0238(7) 0.5652(5) 0.043(2) Uani 1 1 d . . .
C23 C 0.6159(8) 0.5816(6) 0.9750(5) 0.0449(19) Uani 1 1 d . . .
C11 C 0.3849(9) 1.2357(7) 0.7506(5) 0.059(2) Uani 1 1 d . . .
H11 H 0.3869 1.3128 0.7606 0.070 Uiso 1 1 calc R . .
O6 O 0.8531(7) 0.7371(6) 1.0150(5) 0.116(3) Uani 1 1 d . . .
C22 C 0.7382(9) 0.6721(8) 0.9480(7) 0.057(2) Uani 1 1 d . . .
C10 C 0.5192(9) 1.2116(7) 0.7825(5) 0.056(2) Uani 1 1 d . . .
H10 H 0.6137 1.2713 0.8147 0.068 Uiso 1 1 calc R . .
C15 C 0.6582(7) 1.0126(6) 0.5333(5) 0.0352(17) Uani 1 1 d . . .
O1W O 0.8936(8) 0.3629(7) 0.9284(7) 0.192(4) Uani 1 1 d . . .
H1W H 0.9645 0.3324 0.9412 0.289 Uiso 1 1 d RD . .
H2W H 0.8382 0.4023 0.9557 0.289 Uiso 1 1 d RD . .
O2W O 0.9510(11) 0.4985(9) 0.7851(9) 0.254(6) Uani 1 1 d . . .
H3W H 1.0113 0.5669 0.8100 0.382 Uiso 1 1 d RD . .
H4W H 0.9328 0.4567 0.8238 0.382 Uiso 1 1 d RD . .
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
_geom_angle_publ_flag
C29 C28 C27 121.0(6) . 2_877 ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 2_877 . ?
H5W O3W H6W 124.7 . . ?
C14 O2 Zn1 129.7(4) . 2_776 ?
C28 C29 C27 119.9(6) . . ?
C28 C29 H29 120.1 . . ?
C27 C29 H29 120.1 . . ?
C23 C25 C24 120.9(7) 2_667 . ?
C23 C25 H25 119.5 2_667 . ?
C24 C25 H25 119.5 . . ?
C20 C21 C19 120.0(6) . 2_666 ?
C20 C21 H21 120.0 . . ?
C19 C21 H21 120.0 2_666 . ?
C15 C17 C16 120.4(6) 2_676 . ?
C15 C17 H17 119.8 2_676 . ?
C16 C17 H17 119.8 . . ?
C23 C24 C25 120.1(6) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C15 C16 C17 119.6(6) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C1 N1 C5 117.3(6) . . ?
C1 N1 Zn1 126.9(5) . 1_455 ?
C5 N1 Zn1 115.5(5) . 1_455 ?
C12 N2 C13 117.3(7) . . ?
C12 N2 Zn1 128.1(5) . 1_455 ?
C13 N2 Zn1 114.0(5) . 1_455 ?
N2 C13 C9 122.1(7) . . ?
N2 C13 C5 116.2(6) . . ?
C9 C13 C5 121.8(6) . . ?
N1 C5 C4 123.6(7) . . ?
N1 C5 C13 115.8(6) . . ?
C4 C5 C13 120.6(6) . . ?
N1 C1 C2 124.0(7) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 118.5(7) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
O2 Zn1 O1 103.30(17) 2_776 . ?
O2 Zn1 O3 89.28(19) 2_776 . ?
O1 Zn1 O3 85.88(19) . . ?
O2 Zn1 N1 105.54(18) 2_776 1_655 ?
O1 Zn1 N1 151.16(19) . 1_655 ?
O3 Zn1 N1 94.3(2) . 1_655 ?
O2 Zn1 N2 98.24(19) 2_776 1_655 ?
O1 Zn1 N2 98.7(2) . 1_655 ?
O3 Zn1 N2 170.0(2) . 1_655 ?
N1 Zn1 N2 77.4(2) 1_655 1_655 ?
O5 Zn2 O7 134.8(2) . . ?
O5 Zn2 O4 101.5(2) . . ?
O7 Zn2 O4 105.44(19) . . ?
O5 Zn2 N3 110.5(2) . . ?
O7 Zn2 N3 97.4(2) . . ?
O4 Zn2 N3 103.84(19) . . ?
C26 O7 Zn2 119.7(5) . . ?
C7 C6 N3 109.6(6) . . ?
C7 C6 C4 121.0(6) . . ?
N3 C6 C4 129.4(7) . . ?
C14 O1 Zn1 123.6(4) . . ?
C8 N3 C6 103.0(5) . . ?
C8 N3 Zn2 120.5(5) . . ?
C6 N3 Zn2 136.4(5) . . ?
C18 O3 Zn1 113.5(5) . . ?
C8 N4 C7 105.6(6) . . ?
C8 N4 H4 127.2 . . ?
C7 N4 H4 127.2 . . ?
C18 O4 Zn2 158.2(4) . . ?
O3 C18 O4 124.0(7) . . ?
O3 C18 C19 117.6(7) . . ?
O4 C18 C19 118.5(6) . . ?
C22 O5 Zn2 117.7(5) . . ?
C6 C7 N4 105.8(6) . . ?
C6 C7 C9 123.6(6) . . ?
N4 C7 C9 130.6(7) . . ?
N3 C8 N4 116.0(6) . . ?
N3 C8 H8 122.0 . . ?
N4 C8 H8 122.0 . . ?
C2 C3 C4 119.9(7) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C28 C27 C29 119.2(6) 2_877 . ?
C28 C27 C26 120.8(6) 2_877 . ?
C29 C27 C26 120.1(7) . . ?
C13 C9 C10 119.0(7) . . ?
C13 C9 C7 115.8(7) . . ?
C10 C9 C7 125.1(7) . . ?
C5 C4 C3 116.6(7) . . ?
C5 C4 C6 117.1(7) . . ?
C3 C4 C6 126.2(6) . . ?
C21 C20 C19 120.8(6) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
O8 C26 O7 125.0(8) . . ?
O8 C26 C27 119.2(7) . . ?
O7 C26 C27 115.8(8) . . ?
C21 C19 C20 119.2(6) 2_666 . ?
C21 C19 C18 121.7(6) 2_666 . ?
C20 C19 C18 119.1(6) . . ?
N2 C12 C11 123.6(7) . . ?
N2 C12 H12 118.2 . . ?
C11 C12 H12 118.2 . . ?
O1 C14 O2 124.8(6) . . ?
O1 C14 C15 117.6(6) . . ?
O2 C14 C15 117.6(6) . . ?
C25 C23 C24 119.0(6) 2_667 . ?
C25 C23 C22 121.5(7) 2_667 . ?
C24 C23 C22 119.5(7) . . ?
C10 C11 C12 120.0(8) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
O6 C22 O5 124.4(7) . . ?
O6 C22 C23 118.2(7) . . ?
O5 C22 C23 117.4(8) . . ?
C11 C10 C9 118.0(7) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C17 C15 C16 120.0(6) 2_676 . ?
C17 C15 C14 120.8(6) 2_676 . ?
C16 C15 C14 119.1(6) . . ?
H1W O1W H2W 143.8 . . ?
H3W O2W H4W 118.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C28 C29 1.382(9) . ?
C28 C27 1.390(9) 2_877 ?
C28 H28 0.9300 . ?
O3W H5W 0.7499 . ?
O3W H6W 0.8738 . ?
O2 C14 1.261(8) . ?
O2 Zn1 2.028(4) 2_776 ?
C29 C27 1.391(8) . ?
C29 H29 0.9300 . ?
C25 C23 1.375(8) 2_667 ?
C25 C24 1.397(9) . ?
C25 H25 0.9300 . ?
C21 C20 1.382(9) . ?
C21 C19 1.386(8) 2_666 ?
C21 H21 0.9300 . ?
C17 C15 1.379(8) 2_676 ?
C17 C16 1.396(7) . ?
C17 H17 0.9300 . ?
C24 C23 1.381(9) . ?
C24 H24 0.9300 . ?
C16 C15 1.383(9) . ?
C16 H16 0.9300 . ?
N1 C1 1.320(8) . ?
N1 C5 1.339(8) . ?
N1 Zn1 2.119(5) 1_455 ?
N2 C12 1.327(9) . ?
N2 C13 1.365(7) . ?
N2 Zn1 2.123(6) 1_455 ?
C13 C9 1.386(9) . ?
C13 C5 1.467(9) . ?
C5 C4 1.398(8) . ?
C1 C2 1.386(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.357(9) . ?
C2 H2 0.9300 . ?
Zn1 O2 2.028(4) 2_776 ?
Zn1 O1 2.040(4) . ?
Zn1 O3 2.055(5) . ?
Zn1 N1 2.119(5) 1_655 ?
Zn1 N2 2.123(6) 1_655 ?
Zn2 O5 1.924(5) . ?
Zn2 O7 1.925(5) . ?
Zn2 O4 1.974(5) . ?
Zn2 N3 2.013(5) . ?
O7 C26 1.264(8) . ?
C6 C7 1.387(9) . ?
C6 N3 1.413(7) . ?
C6 C4 1.424(9) . ?
O1 C14 1.256(7) . ?
N3 C8 1.317(8) . ?
O3 C18 1.247(7) . ?
N4 C8 1.326(8) . ?
N4 C7 1.404(8) . ?
N4 H4 0.8600 . ?
O4 C18 1.261(7) . ?
C18 C19 1.501(9) . ?
O5 C22 1.247(8) . ?
O8 C26 1.231(9) . ?
C7 C9 1.421(8) . ?
C8 H8 0.9300 . ?
C3 C4 1.404(9) . ?
C3 H3 0.9300 . ?
C27 C28 1.390(9) 2_877 ?
C27 C26 1.514(9) . ?
C9 C10 1.400(9) . ?
C20 C19 1.407(8) . ?
C20 H20 0.9300 . ?
C19 C21 1.386(8) 2_666 ?
C12 C11 1.374(10) . ?
C12 H12 0.9300 . ?
C14 C15 1.502(8) . ?
C23 C25 1.375(8) 2_667 ?
C23 C22 1.511(9) . ?
C11 C10 1.362(9) . ?
C11 H11 0.9300 . ?
O6 C22 1.224(9) . ?
C10 H10 0.9300 . ?
C15 C17 1.379(8) 2_676 ?
O1W H1W 0.8449 . ?
O1W H2W 0.8668 . ?
O2W H3W 0.8331 . ?
O2W H4W 0.8351 . ?
