#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:24:26 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179629 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/93/4509348.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4509348
loop_
_publ_author_name
'Barron, Paul M.'
'Son, Hyun-Tak'
'Hu, Chunhua'
'Choe, Wonyoung'
_publ_section_title
;
 Highly Tunable Heterometallic Frameworks Constructed from Paddle-Wheel
 Units and Metalloporphyrins
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1960
_journal_paper_doi               10.1021/cg801267m
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C58 H32 N6 O9 V Zn2'
_chemical_formula_sum            'C58 H32 N6 O9 V Zn2'
_chemical_formula_weight         1138.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           123
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   16.6901(4)
_cell_length_b                   16.6901(4)
_cell_length_c                   14.0567(7)
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.25
_cell_volume                     3915.6(2)
_computing_cell_refinement       'SAINT+ (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        SAINT+
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART Apex CCD'
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47934
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_correction_T_min  0.8267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             577
_exptl_crystal_size_max          0.516
_exptl_crystal_size_mid          0.476
_exptl_crystal_size_min          0.068
_platon_squeeze_details
;
Disordered, independent solvent molecules were eliminated from the refinement 
using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13].

_refine_ls_R_factor_all           0.0996 
_refine_ls_R_factor_gt            0.0912 
_refine_ls_wR_factor_ref          0.2815 
_refine_ls_wR_factor_gt           0.2681 
;
_refine_diff_density_max         .752
_refine_diff_density_min         -.270
_refine_diff_density_rms         .050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         2265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0358
_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)+(0.0684P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                2048
_reflns_number_total             2265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801267msup3.cif
_cod_data_source_block           c8ch6sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4509348
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, 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
V1 V 0.5000 0.5000 0.46440(10) 0.0615(4) Uani 0.50 8 d SP
Zn1 Zn 0.0000 0.0000 0.39567(2) 0.03748(13) Uani 1 8 d S
O1 O 0.08485(5) 0.08485(5) 0.42135(9) 0.0688(3) Uani 1 2 d S
N1 N 0.37887(11) 0.5000 0.5000 0.0727(7) Uani 1 4 d S
N2 N 0.0000 0.0000 0.25082(18) 0.0540(6) Uani 1 8 d S
C1 C 0.32924(10) 0.43391(10) 0.5000 0.0738(6) Uani 1 2 d S
C2 C 0.24729(10) 0.45966(11) 0.5000 0.0917(8) Uani 1 2 d S
H2 H 0.2024 0.4267 0.5000 0.110 Uiso 1 2 calc SR
C3 C 0.35398(9) 0.35398(9) 0.5000 0.0725(8) Uani 1 4 d S
C4 C 0.29082(9) 0.29082(9) 0.5000 0.0673(7) Uani 1 4 d S
C5 C 0.26089(9) 0.26089(9) 0.41692(18) 0.1041(9) Uani 1 2 d S
H5 H 0.2803 0.2803 0.3594 0.125 Uiso 1 2 calc SR
C6 C 0.20213(8) 0.20213(8) 0.41647(17) 0.0950(8) Uani 1 2 d S
H6 H 0.1827 0.1827 0.3589 0.114 Uiso 1 2 calc SR
C7 C 0.17244(8) 0.17244(8) 0.5000 0.0541(5) Uani 1 4 d S
C8 C 0.10895(8) 0.10895(8) 0.5000 0.0500(5) Uani 1 4 d S
C11 C 0.0000 0.0000 0.0526(2) 0.0665(9) Uani 1 8 d S
C9 C 0.0259(3) 0.0621(3) 0.2020(3) 0.071(3) Uani 0.25 1 d P
H9 H 0.0445 0.1065 0.2354 0.085 Uiso 0.25 1 calc PR
C10 C 0.0269(3) 0.0650(3) 0.1028(3) 0.075(3) Uani 0.25 1 d P
H10 H 0.0455 0.1103 0.0714 0.090 Uiso 0.25 1 calc PR
O2 O 0.5000 0.5000 0.3534(4) 0.0510(10) Uani 0.50 8 d SP
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V .3005 .5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn .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 V1 N1 103.90(4) . .
O2 V1 N1 103.90(4) . 9_666
N1 V1 N1 152.19(8) . 9_666
O2 V1 N1 103.90(4) . 11_566
N1 V1 N1 86.690(18) . 11_566
N1 V1 N1 86.690(18) 9_666 11_566
O2 V1 N1 103.90(4) . 3_655
N1 V1 N1 86.690(18) . 3_655
N1 V1 N1 86.690(18) 9_666 3_655
N1 V1 N1 152.19(8) 11_566 3_655
O1 Zn1 O1 159.57(8) . 2
O1 Zn1 O1 88.197(14) . 4
O1 Zn1 O1 88.198(14) 2 4
O1 Zn1 O1 88.197(14) . 3
O1 Zn1 O1 88.198(14) 2 3
O1 Zn1 O1 159.57(8) 4 3
O1 Zn1 N2 100.22(4) . .
O1 Zn1 N2 100.22(4) 2 .
O1 Zn1 N2 100.22(4) 4 .
O1 Zn1 N2 100.22(4) 3 .
O1 Zn1 Zn1 79.78(4) . 9_556
O1 Zn1 Zn1 79.78(4) 2 9_556
O1 Zn1 Zn1 79.78(4) 4 9_556
O1 Zn1 Zn1 79.78(4) 3 9_556
N2 Zn1 Zn1 180.0 . 9_556
C8 O1 Zn1 127.44(12) . .
C1 N1 C1 106.19(18) . 13_565
C1 N1 V1 125.66(8) . 9_666
C1 N1 V1 125.66(8) 13_565 9_666
C1 N1 V1 125.66(8) . .
C1 N1 V1 125.66(8) 13_565 .
C9 N2 C9 117.1(4) 3 4
C9 N2 C9 117.1(4) 16 15
C9 N2 C9 117.1(4) . 2
C9 N2 C9 117.1(4) 14 13
C9 N2 Zn1 121.5(2) 3 .
C9 N2 Zn1 121.5(2) 16 .
C9 N2 Zn1 121.5(2) . .
C9 N2 Zn1 121.5(2) 4 .
C9 N2 Zn1 121.5(2) 14 .
C9 N2 Zn1 121.5(2) 15 .
C9 N2 Zn1 121.5(2) 2 .
C9 N2 Zn1 121.5(2) 13 .
N1 C1 C3 125.89(16) . .
N1 C1 C2 109.46(15) . .
C3 C1 C2 124.64(16) . .
C2 C2 C1 107.44(10) 13_565 .
C2 C2 H2 126.3 13_565 .
C1 C2 H2 126.3 . .
C1 C3 C1 124.4(2) 7_556 .
C1 C3 C4 117.80(11) 7_556 .
C1 C3 C4 117.80(11) . .
C5 C4 C5 117.7(2) . 10_556
C5 C4 C3 121.17(12) . .
C5 C4 C3 121.17(12) 10_556 .
C4 C5 C6 121.4(2) . .
C4 C5 H5 119.3 . .
C6 C5 H5 119.3 . .
C7 C6 C5 120.6(2) . .
C7 C6 H6 119.7 . .
C5 C6 H6 119.7 . .
C6 C7 C6 118.4(2) . 10_556
C6 C7 C8 120.82(12) . .
C6 C7 C8 120.82(12) 10_556 .
O1 C8 O1 125.6(2) . 10_556
O1 C8 C7 117.23(10) . .
O1 C8 C7 117.22(10) 10_556 .
C10 C11 C10 117.9(4) 4 3
C10 C11 C10 117.9(4) 16 15
C10 C11 C10 117.9(4) . 2
C10 C11 C10 117.9(4) 14 13
C10 C11 C11 121.0(2) 16 9
C10 C11 C11 121.0(2) . 9
C10 C11 C11 121.0(2) 4 9
C10 C11 C11 121.0(2) 14 9
C10 C11 C11 121.0(2) 3 9
C10 C11 C11 121.0(2) 15 9
C10 C11 C11 121.0(2) 2 9
C10 C11 C11 121.0(2) 13 9
N2 C9 C10 123.6(4) . .
N2 C9 H9 118.2 . .
C10 C9 H9 118.2 . .
C11 C10 C9 118.9(4) . .
C11 C10 H10 120.5 . .
C9 C10 H10 120.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O2 1.561(6) .
V1 N1 2.0827(18) .
V1 N1 2.0827(18) 9_666
V1 N1 2.0827(18) 11_566
V1 N1 2.0827(18) 3_655
Zn1 O1 2.0350(11) .
Zn1 O1 2.0351(11) 2
Zn1 O1 2.0351(11) 4
Zn1 O1 2.0351(11) 3
Zn1 N2 2.036(3) .
Zn1 Zn1 2.9332(6) 9_556
O1 C8 1.2434(15) .
N1 C1 1.3794(19) .
N1 C1 1.3794(19) 13_565
N1 V1 2.0827(18) 9_666
N2 C9 1.316(5) 3
N2 C9 1.316(5) 16
N2 C9 1.316(5) .
N2 C9 1.316(5) 4
N2 C9 1.316(5) 14
N2 C9 1.316(5) 15
N2 C9 1.316(5) 2
N2 C9 1.316(5) 13
C1 C3 1.3965(19) .
C1 C2 1.434(2) .
C2 C2 1.346(4) 13_565
C2 H2 0.9300 .
C3 C1 1.3965(19) 7_556
C3 C4 1.491(3) .
C4 C5 1.365(3) .
C4 C5 1.365(3) 10_556
C5 C6 1.387(3) .
C5 H5 0.9300 .
C6 C7 1.367(2) .
C6 H6 0.9300 .
C7 C6 1.367(2) 10_556
C7 C8 1.499(3) .
C8 O1 1.2434(15) 10_556
C11 C10 1.371(5) 16
C11 C10 1.371(5) .
C11 C10 1.371(5) 4
C11 C10 1.371(5) 14
C11 C10 1.371(5) 3
C11 C10 1.371(5) 15
C11 C10 1.371(5) 2
C11 C10 1.371(5) 13
C11 C11 1.478(7) 9
C9 C10 1.394(5) .
C9 H9 0.9300 .
C10 H10 0.9300 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.007 0.326 -0.006 2881.6 687.3
