#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:48:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179541 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/10/4501080.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_4501080
loop_
_publ_author_name
'Farnum, Gregory A.'
'Gandolfo, Chaun M.'
'Supkowski, Ronald M.'
'LaDuca, Robert L.'
_publ_section_title
;
 Divalent Metal Aliphatic Tricarboxylate Dipyridylamine Coordination
 Polymers with New or Rare Binodal Topologies
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4860
_journal_paper_doi               10.1021/cg2006869
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C32 H32 N6 O14 Zn3'
_chemical_formula_weight         920.75
_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
_audit_update_record
;
2011-09-14 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 122.9540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.2048(5)
_cell_length_b                   8.59660(10)
_cell_length_c                   17.9747(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.29
_cell_volume                     3527.37(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15546
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.102
_exptl_absorpt_correction_T_max  0.7296
_exptl_absorpt_correction_T_min  0.6560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3237
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0315P)²+8.1460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                2871
_reflns_number_total             3237
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2006869_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      C2/c
_cod_database_code               4501080
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 0.0000 0.01681(5) 0.2500 0.01554(11) Uani 1 2 d S
Zn2 Zn -0.091542(12) -0.18783(3) -0.039850(18) 0.01977(10) Uani 1 1 d .
O1 O -0.03490(7) -0.1836(2) 0.09383(11) 0.0257(4) Uani 1 1 d .
O1W O 0.23280(9) -0.4716(3) 0.16339(13) 0.0447(6) Uani 1 1 d D
H1WA H 0.2097(12) -0.518(4) 0.175(2) 0.054 Uiso 1 1 d D
H1WB H 0.2681(9) -0.473(4) 0.2083(17) 0.054 Uiso 1 1 d D
O2 O 0.04493(7) -0.1151(2) 0.21943(11) 0.0248(4) Uani 1 1 d .
O3 O 0.07695(8) -0.0253(2) 0.06471(12) 0.0275(4) Uani 1 1 d .
O4 O 0.15433(8) 0.0392(2) 0.19543(13) 0.0292(4) Uani 1 1 d .
O5 O 0.05746(9) -0.6541(3) 0.07411(13) 0.0472(6) Uani 1 1 d .
O6 O 0.14498(8) -0.5745(2) 0.18328(15) 0.0394(5) Uani 1 1 d .
N1 N 0.06616(8) 0.1615(2) 0.33274(13) 0.0178(4) Uani 1 1 d .
N2 N 0.20713(9) 0.4598(3) 0.49233(14) 0.0233(5) Uani 1 1 d D
H2N H 0.2135(12) 0.471(3) 0.5449(13) 0.028 Uiso 1 1 d D
N3 N 0.33631(9) 0.6699(2) 0.46675(13) 0.0193(4) Uani 1 1 d .
C1 C 0.07452(11) 0.2285(3) 0.40670(17) 0.0245(6) Uani 1 1 d .
H1 H 0.0478 0.2056 0.4236 0.029 Uiso 1 1 calc R
C2 C 0.11996(12) 0.3281(3) 0.45833(17) 0.0269(6) Uani 1 1 d .
H2 H 0.1239 0.3733 0.5095 0.032 Uiso 1 1 calc R
C3 C 0.16079(10) 0.3640(3) 0.43620(16) 0.0195(5) Uani 1 1 d .
C4 C 0.15240(11) 0.2934(3) 0.36006(16) 0.0207(5) Uani 1 1 d .
H4 H 0.1789 0.3126 0.3421 0.025 Uiso 1 1 calc R
C5 C 0.10544(11) 0.1959(3) 0.31153(16) 0.0201(5) Uani 1 1 d .
H5 H 0.1003 0.1497 0.2597 0.024 Uiso 1 1 calc R
C6 C 0.34282(11) 0.6456(3) 0.54610(16) 0.0207(5) Uani 1 1 d .
H6 H 0.3787 0.6757 0.5983 0.025 Uiso 1 1 calc R
C7 C 0.30041(10) 0.5800(3) 0.55492(16) 0.0196(5) Uani 1 1 d .
H7 H 0.3068 0.5678 0.6121 0.024 Uiso 1 1 calc R
C8 C 0.24750(10) 0.5309(3) 0.47955(16) 0.0190(5) Uani 1 1 d .
C9 C 0.23897(10) 0.5645(3) 0.39698(16) 0.0197(5) Uani 1 1 d .
H9 H 0.2028 0.5406 0.3437 0.024 Uiso 1 1 calc R
C10 C 0.28366(10) 0.6327(3) 0.39418(16) 0.0200(5) Uani 1 1 d .
H10 H 0.2771 0.6550 0.3377 0.024 Uiso 1 1 calc R
C11 C 0.01913(11) -0.1909(3) 0.14722(16) 0.0206(5) Uani 1 1 d .
C12 C 0.05801(11) -0.2930(3) 0.12972(17) 0.0238(6) Uani 1 1 d .
H12 H 0.0400 -0.2999 0.0643 0.029 Uiso 1 1 calc R
C13 C 0.11986(10) -0.2234(3) 0.17361(17) 0.0214(5) Uani 1 1 d .
H13A H 0.1395 -0.2262 0.2389 0.026 Uiso 1 1 calc R
H13B H 0.1433 -0.2870 0.1579 0.026 Uiso 1 1 calc R
C14 C 0.11752(10) -0.0587(3) 0.14429(17) 0.0223(6) Uani 1 1 d .
C15 C 0.05870(12) -0.4558(3) 0.16543(18) 0.0274(6) Uani 1 1 d .
H15A H 0.0180 -0.4915 0.1406 0.033 Uiso 1 1 calc R
H15B H 0.0790 -0.4519 0.2308 0.033 Uiso 1 1 calc R
C16 C 0.09028(12) -0.5704(3) 0.13959(18) 0.0286(6) Uani 1 1 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
O2 Zn1 O2 108.97(11) . 2
O2 Zn1 N1 126.40(8) . 2
O2 Zn1 N1 96.98(8) 2 2
O2 Zn1 N1 96.98(8) . .
O2 Zn1 N1 126.41(8) 2 .
N1 Zn1 N1 104.04(12) 2 .
O5 Zn2 O3 113.00(10) 5_545 5
O5 Zn2 O1 101.75(8) 5_545 .
O3 Zn2 O1 97.73(8) 5 .
O5 Zn2 N3 136.03(10) 5_545 8_455
O3 Zn2 N3 105.16(8) 5 8_455
O1 Zn2 N3 93.72(7) . 8_455
C11 O1 Zn2 136.81(17) . .
H1WA O1W H1WB 111(3) . .
C11 O2 Zn1 120.22(15) . .
C14 O3 Zn2 107.73(17) . 5
C16 O5 Zn2 119.13(18) . 5_545
C5 N1 C1 116.7(2) . .
C5 N1 Zn1 116.89(16) . .
C1 N1 Zn1 126.36(16) . .
C3 N2 C8 129.5(2) . .
C3 N2 H2N 115.1(19) . .
C8 N2 H2N 115.2(19) . .
C10 N3 C6 116.3(2) . .
C10 N3 Zn2 120.76(16) . 8_556
C6 N3 Zn2 119.68(16) . 8_556
N1 C1 C2 122.7(2) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C1 C2 C3 120.5(2) . .
C1 C2 H2 119.7 . .
C3 C2 H2 119.7 . .
N2 C3 C4 125.0(2) . .
N2 C3 C2 118.3(2) . .
C4 C3 C2 116.7(2) . .
C5 C4 C3 119.2(2) . .
C5 C4 H4 120.4 . .
C3 C4 H4 120.4 . .
N1 C5 C4 124.1(2) . .
N1 C5 H5 117.9 . .
C4 C5 H5 117.9 . .
N3 C6 C7 123.4(2) . .
N3 C6 H6 118.3 . .
C7 C6 H6 118.3 . .
C6 C7 C8 120.0(2) . .
C6 C7 H7 120.0 . .
C8 C7 H7 120.0 . .
N2 C8 C7 117.7(2) . .
N2 C8 C9 125.4(2) . .
C7 C8 C9 116.9(2) . .
C10 C9 C8 119.1(2) . .
C10 C9 H9 120.5 . .
C8 C9 H9 120.5 . .
N3 C10 C9 124.1(2) . .
N3 C10 H10 118.0 . .
C9 C10 H10 118.0 . .
O1 C11 O2 121.8(2) . .
O1 C11 C12 121.8(2) . .
O2 C11 C12 116.4(2) . .
C11 C12 C15 106.8(2) . .
C11 C12 C13 110.8(2) . .
C15 C12 C13 112.3(2) . .
C11 C12 H12 108.9 . .
C15 C12 H12 108.9 . .
C13 C12 H12 108.9 . .
C14 C13 C12 111.2(2) . .
C14 C13 H13A 109.4 . .
C12 C13 H13A 109.4 . .
C14 C13 H13B 109.4 . .
C12 C13 H13B 109.4 . .
H13A C13 H13B 108.0 . .
O4 C14 O3 122.2(3) . .
O4 C14 C13 121.0(2) . .
O3 C14 C13 116.9(2) . .
C12 C15 C16 109.9(2) . .
C12 C15 H15A 109.7 . .
C16 C15 H15A 109.7 . .
C12 C15 H15B 109.7 . .
C16 C15 H15B 109.7 . .
H15A C15 H15B 108.2 . .
O5 C16 O6 124.9(3) . .
O5 C16 C15 115.1(2) . .
O6 C16 C15 120.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 1.9528(17) .
Zn1 O2 1.9528(17) 2
Zn1 N1 2.021(2) 2
Zn1 N1 2.022(2) .
Zn2 O5 1.9250(19) 5_545
Zn2 O3 1.9764(19) 5
Zn2 O1 2.0301(17) .
Zn2 N3 2.036(2) 8_455
O1 C11 1.245(3) .
O1W H1WA 0.858(18) .
O1W H1WB 0.855(18) .
O2 C11 1.269(3) .
O3 C14 1.276(3) .
O3 Zn2 1.9764(19) 5
O4 C14 1.247(3) .
O5 C16 1.248(3) .
O5 Zn2 1.9251(19) 5_545
O6 C16 1.249(3) .
N1 C5 1.348(3) .
N1 C1 1.350(3) .
N2 C3 1.379(3) .
N2 C8 1.381(3) .
N2 H2N 0.870(17) .
N3 C10 1.350(3) .
N3 C6 1.354(3) .
N3 Zn2 2.035(2) 8_556
C1 C2 1.369(4) .
C1 H1 0.9500 .
C2 C3 1.403(3) .
C2 H2 0.9500 .
C3 C4 1.398(3) .
C4 C5 1.372(3) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C7 1.369(4) .
C6 H6 0.9500 .
C7 C8 1.401(3) .
C7 H7 0.9500 .
C8 C9 1.402(3) .
C9 C10 1.375(3) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 C12 1.533(4) .
C12 C15 1.535(4) .
C12 C13 1.539(3) .
C12 H12 1.0000 .
C13 C14 1.500(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C15 C16 1.535(4) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O6 0.858(18) 1.911(19) 2.747(3) 165(3) .
O1W H1WB O4 0.855(18) 1.867(18) 2.720(3) 175(4) 4_545
N2 H2N O1W 0.870(17) 1.895(18) 2.760(3) 173(3) 6_556
