#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/93/4509349.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_4509349
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         'C68 H40 Mn N8 O8 Zn2, (N O3)'
_chemical_formula_sum            'C68 H40 Mn N9 O11 Zn2'
_chemical_formula_weight         1344.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 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            2
_cell_length_a                   16.6609(11)
_cell_length_b                   16.6609(11)
_cell_length_c                   25.688(2)
_cell_measurement_reflns_used    6232
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.80
_cell_measurement_theta_min      2.35
_cell_volume                     7130.6(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'omega 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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20077
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.9563
_exptl_absorpt_correction_T_min  0.8092
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_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].

R factors before data are squeezed:
_refine_ls_R_factor_all           0.1497 
_refine_ls_R_factor_gt            0.1142 
_refine_ls_wR_factor_ref          0.4113 
_refine_ls_wR_factor_gt           0.3597 
;
_refine_diff_density_max         1.578
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2033
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0811
_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)+(0.1891P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2219
_refine_ls_wR_factor_ref         0.2368
_reflns_number_gt                1501
_reflns_number_total             2033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801267msup4.cif
_cod_data_source_block           C7CH10sq
_cod_original_sg_symbol_Hall     '-I 4 2 '
_cod_database_code               4509349
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+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-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+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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 0.5000 0.5000 0.05633(3) 0.0364(4) Uani 1 8 d S
Mn1 Mn 0.0000 0.0000 0.0000 0.0311(4) Uani 1 16 d S
O1 O 0.41557(14) 0.41557(14) 0.04233(15) 0.0832(14) Uani 1 2 d S
N1 N 0.0000 0.1208(3) 0.0000 0.0355(10) Uani 1 4 d S
C1 C 0.0659(2) 0.1708(2) 0.0000 0.0414(9) Uani 1 2 d S
C2 C 0.0402(3) 0.2527(2) 0.0000 0.0506(11) Uani 1 2 d S
H2 H 0.0739 0.2987 0.0000 0.061 Uiso 1 2 calc SR
C3 C 0.1465(2) 0.1465(2) 0.0000 0.0418(13) Uani 1 4 d S
C4 C 0.2092(2) 0.2092(2) 0.0000 0.0434(13) Uani 1 4 d S
C5 C 0.2388(2) 0.2388(2) 0.0451(2) 0.086(2) Uani 1 2 d S
H5 H 0.2187 0.2187 0.0772 0.103 Uiso 1 2 calc SR
C6 C 0.2975(2) 0.2975(2) 0.0459(2) 0.086(2) Uani 1 2 d S
H6 H 0.3171 0.3171 0.0783 0.103 Uiso 1 2 calc SR
C7 C 0.3278(2) 0.3278(2) 0.0000 0.0399(12) Uani 1 4 d S
C8 C 0.3913(3) 0.3913(3) 0.0000 0.0422(13) Uani 1 4 d S
N2 N 0.0000 0.0000 0.0913(3) 0.052(2) Uani 1 8 d SD
N3 N 0.0000 0.0000 0.3650(3) 0.0437(16) Uani 1 8 d SD
C11 C 0.0000 0.0000 0.1980(3) 0.048(2) Uani 1 8 d SD
C12 C 0.0000 0.0000 0.2568(3) 0.050(2) Uani 1 8 d SD
C9 C 0.0273(7) 0.0635(6) 0.1183(4) 0.062(5) Uani 0.25 1 d PDU
H9 H 0.0476 0.1084 0.0996 0.074 Uiso 0.25 1 calc PR
C10 C 0.0272(7) 0.0663(6) 0.1722(3) 0.058(5) Uani 0.25 1 d PDU
H10 H 0.0453 0.1125 0.1905 0.070 Uiso 0.25 1 calc PR
C13 C 0.0307(9) 0.0636(7) 0.2851(3) 0.063(7) Uani 0.25 1 d PDU
H13 H 0.0523 0.1088 0.2675 0.076 Uiso 0.25 1 calc PR
C14 C 0.0300(8) 0.0617(8) 0.3378(3) 0.067(8) Uani 0.25 1 d PDU
H14 H 0.0518 0.1060 0.3563 0.080 Uiso 0.25 1 calc PR
N4 N 0.2790(18) 0.0000 0.1433(12) 0.120 Uiso 0.13 2 d SPD
O2 O 0.2429(17) 0.0635(3) 0.1435(12) 0.120 Uiso 0.13 1 d PD
O3 O 0.3522(17) 0.0000 0.1422(15) 0.120 Uiso 0.13 2 d SPD
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'
Mn Mn 0.3368 0.7283 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0410
0.00 0.00 -1.00 0.0450
1.00 0.00 0.00 0.2220
-1.00 0.00 0.00 0.2360
0.00 1.00 0.00 0.1210
0.00 -1.00 0.00 0.1320
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
N3 Zn1 O1 100.25(11) 25 .
N3 Zn1 O1 100.25(11) 25 4_565
O1 Zn1 O1 88.19(4) . 4_565
N3 Zn1 O1 100.25(11) 25 2_665
O1 Zn1 O1 159.5(2) . 2_665
O1 Zn1 O1 88.19(4) 4_565 2_665
N3 Zn1 O1 100.25(11) 25 3_655
O1 Zn1 O1 88.19(4) . 3_655
O1 Zn1 O1 159.5(2) 4_565 3_655
O1 Zn1 O1 88.19(4) 2_665 3_655
N3 Zn1 Zn1 180.0 25 17_665
O1 Zn1 Zn1 79.75(11) . 17_665
O1 Zn1 Zn1 79.75(11) 4_565 17_665
O1 Zn1 Zn1 79.75(11) 2_665 17_665
O1 Zn1 Zn1 79.75(11) 3_655 17_665
N1 Mn1 N1 90.0 3 .
N1 Mn1 N1 90.0 3 17
N1 Mn1 N1 180.0 . 17
N1 Mn1 N1 180.0 3 19
N1 Mn1 N1 90.0 . 19
N1 Mn1 N1 90.0 17 19
N1 Mn1 N2 90.0 3 17
N1 Mn1 N2 90.0 . 17
N1 Mn1 N2 90.0 17 17
N1 Mn1 N2 90.0 19 17
N1 Mn1 N2 90.0 3 .
N1 Mn1 N2 90.0 . .
N1 Mn1 N2 90.0 17 .
N1 Mn1 N2 90.0 19 .
N2 Mn1 N2 180.0 17 .
C8 O1 Zn1 128.0(4) . .
C1 N1 C1 105.7(5) . 5
C1 N1 Mn1 127.1(2) . .
C1 N1 Mn1 127.1(2) 5 .
N1 C1 C3 126.1(4) . .
N1 C1 C2 109.7(4) . .
C3 C1 C2 124.2(4) . .
C2 C2 C1 107.5(3) 5 .
C2 C2 H2 126.3 5 .
C1 C2 H2 126.3 . .
C1 C3 C1 123.5(5) 7 .
C1 C3 C4 118.2(3) 7 .
C1 C3 C4 118.2(3) . .
C5 C4 C5 118.0(6) . 18
C5 C4 C3 121.0(3) . .
C5 C4 C3 121.0(3) 18 .
C4 C5 C6 121.9(5) . .
C4 C5 H5 119.1 . .
C6 C5 H5 119.1 . .
C7 C6 C5 120.3(5) . .
C7 C6 H6 119.9 . .
C5 C6 H6 119.9 . .
C6 C7 C6 117.7(6) 18 .
C6 C7 C8 121.2(3) 18 .
C6 C7 C8 121.2(3) . .
O1 C8 O1 124.6(6) . 18
O1 C8 C7 117.7(3) . .
O1 C8 C7 117.7(3) 18 .
C9 N2 C9 117.9(11) 24 23
C9 N2 C9 117.9(11) . 2
C9 N2 C9 117.9(11) 22 21
C9 N2 C9 117.9(11) 4 3
C9 N2 Mn1 121.0(6) 24 .
C9 N2 Mn1 121.0(6) . .
C9 N2 Mn1 121.0(6) 23 .
C9 N2 Mn1 121.0(6) 22 .
C9 N2 Mn1 121.0(6) 4 .
C9 N2 Mn1 121.0(6) 2 .
C9 N2 Mn1 121.0(6) 21 .
C9 N2 Mn1 121.0(6) 3 .
C14 N3 C14 117.3(10) 23 24
C14 N3 C14 117.3(10) 2 .
C14 N3 C14 117.3(10) 3 4
C14 N3 C14 117.3(10) 21 22
C14 N3 Zn1 121.4(5) 23 25
C14 N3 Zn1 121.4(5) 2 25
C14 N3 Zn1 121.4(5) 21 25
C14 N3 Zn1 121.4(5) 3 25
C14 N3 Zn1 121.4(5) 24 25
C14 N3 Zn1 121.4(5) . 25
C14 N3 Zn1 121.4(5) 4 25
C14 N3 Zn1 121.4(5) 22 25
C10 C11 C10 121.9(10) 2 .
C10 C11 C10 121.9(10) 24 23
C10 C11 C10 121.9(10) 3 4
C10 C11 C10 121.9(10) 21 22
C10 C11 C12 119.1(5) 2 .
C10 C11 C12 119.1(5) 3 .
C10 C11 C12 119.1(5) 21 .
C10 C11 C12 119.1(5) . .
C10 C11 C12 119.1(5) 24 .
C10 C11 C12 119.1(5) 23 .
C10 C11 C12 119.1(5) 4 .
C10 C11 C12 119.1(5) 22 .
C13 C12 C13 116.6(10) . 2
C13 C12 C13 116.6(10) 24 23
C13 C12 C13 116.6(10) 4 3
C13 C12 C13 116.6(10) 22 21
C13 C12 C11 121.7(5) 24 .
C13 C12 C11 121.7(5) . .
C13 C12 C11 121.7(5) 2 .
C13 C12 C11 121.7(5) 23 .
C13 C12 C11 121.7(5) 22 .
C13 C12 C11 121.7(5) 4 .
C13 C12 C11 121.7(5) 3 .
C13 C12 C11 121.7(5) 21 .
N2 C9 C10 122.8(10) . .
N2 C9 H9 118.6 . .
C10 C9 H9 118.6 . .
C11 C10 C9 117.3(9) . .
C11 C10 H10 121.3 . .
C9 C10 H10 121.3 . .
C14 C13 C12 120.3(9) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
N3 C14 C13 122.8(9) . .
N3 C14 H14 118.6 . .
C13 C14 H14 118.6 . .
O2 N4 O2 120.8(11) 21 .
O2 N4 O3 119.6(5) 21 .
O2 N4 O3 119.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N3 2.021(7) 25
Zn1 O1 2.022(3) .
Zn1 O1 2.022(3) 4_565
Zn1 O1 2.022(3) 2_665
Zn1 O1 2.022(3) 3_655
Zn1 Zn1 2.8940(18) 17_665
Mn1 N1 2.013(4) 3
Mn1 N1 2.013(4) .
Mn1 N1 2.013(4) 17
Mn1 N1 2.013(4) 19
Mn1 N2 2.346(8) 17
Mn1 N2 2.346(8) .
O1 C8 1.228(5) .
N1 C1 1.378(5) .
N1 C1 1.378(5) 5
C1 C3 1.402(5) .
C1 C2 1.431(6) .
C2 C2 1.339(9) 5
C2 H2 0.9500 .
C3 C1 1.402(5) 7
C3 C4 1.478(8) .
C4 C5 1.353(6) .
C4 C5 1.353(6) 18
C5 C6 1.383(7) .
C5 H5 0.9500 .
C6 C7 1.379(6) .
C6 H6 0.9500 .
C7 C6 1.379(6) 18
C7 C8 1.496(8) .
C8 O1 1.228(5) 18
N2 C9 1.345(8) 24
N2 C9 1.345(8) .
N2 C9 1.345(8) 23
N2 C9 1.345(8) 22
N2 C9 1.345(8) 4
N2 C9 1.345(8) 2
N2 C9 1.345(8) 21
N2 C9 1.345(8) 3
N3 C14 1.339(8) 23
N3 C14 1.339(8) 2
N3 C14 1.339(8) 21
N3 C14 1.339(8) 3
N3 C14 1.339(8) 24
N3 C14 1.339(8) .
N3 C14 1.339(8) 4
N3 C14 1.339(8) 22
N3 Zn1 2.021(7) 25
C11 C10 1.366(8) 2
C11 C10 1.366(8) 3
C11 C10 1.366(8) 21
C11 C10 1.366(8) .
C11 C10 1.366(8) 24
C11 C10 1.366(8) 23
C11 C10 1.366(8) 4
C11 C10 1.366(8) 22
C11 C12 1.509(11) .
C12 C13 1.383(8) 24
C12 C13 1.383(8) .
C12 C13 1.383(8) 2
C12 C13 1.383(8) 23
C12 C13 1.383(8) 22
C12 C13 1.383(8) 4
C12 C13 1.383(8) 3
C12 C13 1.383(8) 21
C9 C10 1.385(8) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C13 C14 1.356(8) .
C13 H13 0.9500 .
C14 H14 0.9500 .
N4 O2 1.217(6) 21
N4 O2 1.217(6) .
N4 O3 1.220(9) .
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 -0.025 0.309 0.434 3640.3 682.4
