#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/93/4509347.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_4509347
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 Co2, (N O3)'
_chemical_formula_sum            'C68 H40 Co2 Mn N9 O11'
_chemical_formula_weight         1331.89
_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                   16.6905(12)
_cell_length_b                   16.6905(12)
_cell_length_c                   25.466(4)
_cell_measurement_reflns_used    5119
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.54
_cell_measurement_theta_min      2.35
_cell_volume                     7094.1(13)
_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      100(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_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  0.0959
_diffrn_reflns_av_sigmaI/netI    0.0469
_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       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23724
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.9794
_exptl_absorpt_correction_T_min  0.8109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    0.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_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           0.1991 
_refine_ls_R_factor_gt            0.1410 
_refine_ls_wR_factor_ref          0.4396 
_refine_ls_wR_factor_gt           0.3909 
;
_refine_diff_density_max         2.590
_refine_diff_density_min         -.529
_refine_diff_density_rms         .164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2009
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0967
_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)+(0.1848P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2416
_refine_ls_wR_factor_ref         0.2596
_reflns_number_gt                1309
_reflns_number_total             2009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801267msup2.cif
_cod_data_source_block           c7ch40-p2b3804sq
_cod_original_cell_volume        7094.3(13)
_cod_original_sg_symbol_Hall     '-I 4 2 '
_cod_database_code               4509347
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
Co1 Co 0.5000 0.5000 0.05141(5) 0.0290(5) Uani 1 8 d S
Mn1 Mn 0.0000 0.0000 0.0000 0.0258(5) Uani 1 16 d S
O1 O 0.41491(17) 0.41491(17) 0.04355(15) 0.0605(13) Uani 1 2 d S
N1 N 0.0000 0.1205(3) 0.0000 0.0288(12) Uani 1 4 d S
C1 C 0.0651(3) 0.1700(3) 0.0000 0.0348(12) Uani 1 2 d S
C2 C 0.0401(3) 0.2531(3) 0.0000 0.0477(15) Uani 1 2 d S
H2 H 0.0740 0.2988 0.0000 0.057 Uiso 1 2 calc SR
C3 C 0.1460(3) 0.1460(3) 0.0000 0.0389(17) Uani 1 4 d SD
C4 C 0.2094(3) 0.2094(3) 0.0000 0.0419(18) Uani 1 4 d SD
C5 C 0.2392(3) 0.2392(3) 0.0456(2) 0.072(2) Uani 1 2 d S
H5 H 0.2193 0.2193 0.0781 0.086 Uiso 1 2 calc SR
C6 C 0.2982(3) 0.2982(3) 0.0457(2) 0.070(2) Uani 1 2 d S
H6 H 0.3182 0.3182 0.0781 0.084 Uiso 1 2 calc SR
C7 C 0.3271(3) 0.3271(3) 0.0000 0.0430(18) Uani 1 4 d SD
C8 C 0.3913(3) 0.3913(3) 0.0000 0.0447(19) Uani 1 4 d SD
N2 N 0.0000 0.0000 0.0918(3) 0.0245(16) Uani 1 8 d SD
N3 N 0.0000 0.0000 0.3667(4) 0.039(2) Uani 1 8 d SD
C11 C 0.0000 0.0000 0.2018(5) 0.045(3) Uani 1 8 d SD
C12 C 0.0000 0.0000 0.2570(5) 0.049(3) Uani 1 8 d SD
C9 C 0.0151(13) 0.0674(6) 0.1180(4) 0.050(6) Uani 0.25 1 d PDU
H9 H 0.0263 0.1152 0.0992 0.061 Uiso 0.25 1 calc PR
C10 C 0.0147(14) 0.0685(7) 0.1723(4) 0.053(6) Uani 0.25 1 d PDU
H10 H 0.0248 0.1176 0.1900 0.063 Uiso 0.25 1 calc PR
C13 C 0.0335(10) 0.0620(8) 0.2865(4) 0.065(7) Uani 0.25 1 d PDU
H13 H 0.0585 0.1052 0.2686 0.078 Uiso 0.25 1 calc PR
C14 C 0.0317(9) 0.0633(8) 0.3415(4) 0.060(7) Uani 0.25 1 d PDU
H14 H 0.0524 0.1077 0.3605 0.072 Uiso 0.25 1 calc PR
N4 N 0.2804(19) 0.0000 0.1461(13) 0.120 Uiso 0.12 2 d SPD
O2 O 0.2448(19) 0.0632(3) 0.1502(15) 0.120 Uiso 0.13 1 d PD
O3 O 0.3527(19) 0.0000 0.1383(18) 0.120 Uiso 0.12 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 .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'
Mn Mn .3368 .7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co .3494 .9721 '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
O1 Co1 O1 168.6(2) . 2_665
O1 Co1 O1 89.44(2) . 4_565
O1 Co1 O1 89.44(2) 2_665 4_565
O1 Co1 O1 89.44(2) . 3_655
O1 Co1 O1 89.44(2) 2_665 3_655
O1 Co1 O1 168.6(2) 4_565 3_655
O1 Co1 N3 95.69(12) . 25
O1 Co1 N3 95.69(12) 2_665 25
O1 Co1 N3 95.69(12) 4_565 25
O1 Co1 N3 95.69(12) 3_655 25
O1 Co1 Co1 84.31(12) . 17_665
O1 Co1 Co1 84.31(12) 2_665 17_665
O1 Co1 Co1 84.31(12) 4_565 17_665
O1 Co1 Co1 84.31(12) 3_655 17_665
N3 Co1 Co1 180.0 25 17_665
N1 Mn1 N1 180.0 19 3
N1 Mn1 N1 90.0 19 17
N1 Mn1 N1 90.0 3 17
N1 Mn1 N1 90.0 19 .
N1 Mn1 N1 90.0 3 .
N1 Mn1 N1 180.0 17 .
N1 Mn1 N2 90.0 19 17
N1 Mn1 N2 90.0 3 17
N1 Mn1 N2 90.0 17 17
N1 Mn1 N2 90.0 . 17
N1 Mn1 N2 90.0 19 .
N1 Mn1 N2 90.0 3 .
N1 Mn1 N2 90.0 17 .
N1 Mn1 N2 90.0 . .
N2 Mn1 N2 180.0 17 .
C8 O1 Co1 122.4(4) . .
C1 N1 C1 105.6(5) . 5
C1 N1 Mn1 127.2(3) . .
C1 N1 Mn1 127.2(3) 5 .
N1 C1 C3 126.2(4) . .
N1 C1 C2 110.5(4) . .
C3 C1 C2 123.3(4) . .
C2 C2 C1 106.8(3) 5 .
C2 C2 H2 126.6 5 .
C1 C2 H2 126.6 . .
C1 C3 C1 123.1(6) 7 .
C1 C3 C4 118.5(3) 7 .
C1 C3 C4 118.5(3) . .
C5 C4 C5 117.6(7) 18 .
C5 C4 C3 121.2(3) 18 .
C5 C4 C3 121.2(3) . .
C4 C5 C6 121.3(6) . .
C4 C5 H5 119.3 . .
C6 C5 H5 119.3 . .
C7 C6 C5 120.2(6) . .
C7 C6 H6 119.9 . .
C5 C6 H6 119.9 . .
C6 C7 C6 119.3(7) 18 .
C6 C7 C8 120.4(4) 18 .
C6 C7 C8 120.4(4) . .
O1 C8 O1 126.6(7) . 18
O1 C8 C7 116.7(3) . .
O1 C8 C7 116.7(3) 18 .
C9 N2 C9 119.8(11) 2 .
C9 N2 C9 119.8(11) 23 24
C9 N2 C9 119.8(11) 21 22
C9 N2 C9 119.8(11) 4 3
C9 N2 Mn1 120.1(6) 23 .
C9 N2 Mn1 120.1(6) 2 .
C9 N2 Mn1 120.1(6) 21 .
C9 N2 Mn1 120.1(6) . .
C9 N2 Mn1 120.1(6) 24 .
C9 N2 Mn1 120.1(6) 22 .
C9 N2 Mn1 120.1(6) 4 .
C9 N2 Mn1 120.1(6) 3 .
C14 N3 C14 123.0(13) 2 .
C14 N3 C14 123.0(13) 23 24
C14 N3 C14 123.0(13) 21 22
C14 N3 C14 123.0(13) 3 4
C14 N3 Co1 118.5(6) 2 25
C14 N3 Co1 118.5(6) 21 25
C14 N3 Co1 118.5(6) 23 25
C14 N3 Co1 118.5(6) 3 25
C14 N3 Co1 118.5(6) . 25
C14 N3 Co1 118.5(6) 24 25
C14 N3 Co1 118.5(6) 22 25
C14 N3 Co1 118.5(6) 4 25
C10 C11 C10 114.5(14) 2 .
C10 C11 C10 114.5(14) 23 24
C10 C11 C10 114.5(14) 21 22
C10 C11 C10 114.5(14) 3 4
C10 C11 C12 122.7(7) 23 .
C10 C11 C12 122.7(7) 2 .
C10 C11 C12 122.7(7) 21 .
C10 C11 C12 122.7(7) 3 .
C10 C11 C12 122.7(7) . .
C10 C11 C12 122.7(7) 24 .
C10 C11 C12 122.7(7) 22 .
C10 C11 C12 122.7(7) 4 .
C13 C12 C13 114.8(14) 4 3
C13 C12 C13 114.8(14) 24 23
C13 C12 C13 114.8(14) . 2
C13 C12 C13 114.8(14) 22 21
C13 C12 C11 122.6(7) 24 .
C13 C12 C11 122.6(7) . .
C13 C12 C11 122.6(7) 4 .
C13 C12 C11 122.6(7) 22 .
C13 C12 C11 122.6(7) 3 .
C13 C12 C11 122.6(7) 23 .
C13 C12 C11 122.6(7) 2 .
C13 C12 C11 122.6(7) 21 .
N2 C9 C10 120.8(10) . .
N2 C9 H9 119.6 . .
C10 C9 H9 119.6 . .
C9 C10 C11 122.0(11) . .
C9 C10 H10 119.0 . .
C11 C10 H10 119.0 . .
C12 C13 C14 122.8(12) . .
C12 C13 H13 118.6 . .
C14 C13 H13 118.6 . .
N3 C14 C13 118.3(11) . .
N3 C14 H14 120.9 . .
C13 C14 H14 120.9 . .
O2 N4 O2 120.4(11) 21 .
O2 N4 O3 119.8(5) 21 .
O2 N4 O3 119.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.018(4) .
Co1 O1 2.018(4) 2_665
Co1 O1 2.018(4) 4_565
Co1 O1 2.018(4) 3_655
Co1 N3 2.086(9) 25
Co1 Co1 2.618(3) 17_665
Mn1 N1 2.011(5) 19
Mn1 N1 2.011(5) 3
Mn1 N1 2.011(5) 17
Mn1 N1 2.011(5) .
Mn1 N2 2.338(8) 17
Mn1 N2 2.338(8) .
O1 C8 1.241(5) .
N1 C1 1.365(5) .
N1 C1 1.365(5) 5
C1 C3 1.408(5) .
C1 C2 1.449(6) .
C2 C2 1.337(10) 5
C2 H2 0.9500 .
C3 C1 1.408(5) 7
C3 C4 1.497(7) .
C4 C5 1.357(6) 18
C4 C5 1.357(6) .
C5 C6 1.394(9) .
C5 H5 0.9500 .
C6 C7 1.350(6) .
C6 H6 0.9500 .
C7 C6 1.350(6) 18
C7 C8 1.515(7) .
C8 O1 1.241(5) 18
N2 C9 1.332(8) 23
N2 C9 1.332(8) 2
N2 C9 1.332(8) 21
N2 C9 1.332(8) .
N2 C9 1.332(8) 24
N2 C9 1.332(8) 22
N2 C9 1.332(8) 4
N2 C9 1.332(8) 3
N3 C14 1.345(8) 2
N3 C14 1.345(8) 21
N3 C14 1.345(8) 23
N3 C14 1.345(8) 3
N3 C14 1.345(8) .
N3 C14 1.345(8) 24
N3 C14 1.345(8) 22
N3 C14 1.345(8) 4
N3 Co1 2.086(9) 25
C11 C10 1.391(8) 23
C11 C10 1.391(8) 2
C11 C10 1.391(8) 21
C11 C10 1.391(8) 3
C11 C10 1.391(8) .
C11 C10 1.391(8) 24
C11 C10 1.391(8) 22
C11 C10 1.391(8) 4
C11 C12 1.405(19) .
C12 C13 1.396(9) 24
C12 C13 1.396(9) .
C12 C13 1.396(9) 4
C12 C13 1.396(9) 22
C12 C13 1.396(9) 3
C12 C13 1.396(9) 23
C12 C13 1.396(9) 2
C12 C13 1.396(9) 21
C9 C10 1.382(9) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C13 C14 1.400(9) .
C13 H13 0.9500 .
C14 H14 0.9500 .
N4 O2 1.215(6) 21
N4 O2 1.215(6) .
N4 O3 1.222(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 -0.021 0.309 0.435 3611.1 448.8
