#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/16/4321616.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_4321616
loop_
_publ_author_name
'Michael Harmjanz'
'Michael J. Scott'
_publ_contact_author_address
;
 Department of Chemistry, University of Florida, Gainesville, FL 32611-7200, 
;
_publ_contact_author_email       mjscott@chem.ufl.edu
_publ_contact_author_fax         '(352) 392-3255'
_publ_contact_author_phone       '(352) 846-1165'
_publ_section_title
;
 Facile Synthesis of Stacked, Heteronuclear Porphyrin Arrays with Varied
 Architectures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5428
_journal_page_last               5429
_journal_paper_doi               10.1021/ic0010656
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C72.5 H86 Cu Mn N4 O22.5'
_chemical_formula_weight         1491.93
_chemical_name_common            '[CuMethoxyporphyrin]2- [Mn(HOMe)6]2+ '
_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                95.221(2)
_cell_angle_beta                 94.625(2)
_cell_angle_gamma                108.9330(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9439(9)
_cell_length_b                   14.1435(11)
_cell_length_c                   14.3367(11)
_cell_measurement_temperature    173(2)
_cell_volume                     2076.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11338
_diffrn_reflns_theta_full        24.74
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.655170
_exptl_absorpt_correction_type   'Corrected by SADABS'
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             783
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0061(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0735
_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)+(0.1335P)²+0.2022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2289
_reflns_number_gt                4564
_reflns_number_total             7063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0010656_3.cif
_cod_data_source_block           6-[CuMethoxyporphyrin]2-[Mn(HOMe)6]2+
_cod_original_formula_sum        'C72.50 H86 Cu Mn N4 O22.50'
_cod_database_code               4321616
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
Cu1 Cu -0.5000 0.5000 0.5000 0.0245(3) Uani 1 2 d S . .
Mn1 Mn 0.0000 0.5000 0.5000 0.0365(3) Uani 1 2 d S . .
O1 O -0.2152(4) 0.5261(3) 0.2590(3) 0.0514(11) Uani 1 1 d . . .
O2 O -0.1593(4) 0.6729(3) 0.3504(3) 0.0447(10) Uani 1 1 d . . .
O3 O -0.9629(4) 0.0164(4) 0.1362(4) 0.0747(16) Uani 1 1 d . . .
O4 O -0.7839(4) -0.0474(3) 0.0562(3) 0.0612(13) Uani 1 1 d . . .
O5 O -0.5335(4) 0.0511(3) 0.0977(2) 0.0395(9) Uani 1 1 d . . .
O6 O 0.0833(5) 0.3826(4) 0.4927(3) 0.0633(13) Uani 1 1 d . . .
H6 H 0.0920 0.3643 0.5463 0.095 Uiso 1 1 calc R . .
O7 O -0.1432(4) 0.4262(3) 0.3829(3) 0.0630(13) Uani 1 1 d . . .
H7 H -0.1617 0.4663 0.3492 0.095 Uiso 1 1 calc R . .
O8 O 0.1199(4) 0.5852(5) 0.4019(4) 0.0781(16) Uani 1 1 d . . .
H8A H 0.1091 0.6368 0.3831 0.117 Uiso 1 1 calc R . .
O9 O -0.0622(9) 0.3319(9) 0.1123(9) 0.140(4) Uani 0.75 1 d P . .
H9 H -0.1337 0.3292 0.1313 0.211 Uiso 0.75 1 calc PR . .
O10 O -0.0199(9) 0.8645(6) 0.3944(7) 0.107(3) Uani 0.75 1 d P . .
H10 H -0.0689 0.8077 0.3686 0.161 Uiso 0.75 1 calc PR . .
O11 O -0.1877(10) 1.2067(7) 0.5922(10) 0.088(4) Uani 0.50 1 d P . .
O12 O -0.2871(5) 0.3810(4) 0.1078(4) 0.0751(15) Uani 1 1 d . . .
H12 H -0.2684 0.4325 0.1475 0.113 Uiso 1 1 calc R . .
O13 O -0.391(4) 1.049(3) 0.386(3) 0.151(12) Uiso 0.25 1 d P . .
N1 N -0.5196(4) 0.4802(3) 0.3591(3) 0.0269(9) Uani 1 1 d . . .
N2 N -0.4274(4) 0.6488(3) 0.4983(3) 0.0257(9) Uani 1 1 d . . .
C1 C -0.6599(5) 0.1802(4) 0.4537(4) 0.0360(12) Uani 1 1 d . . .
H1A H -0.6924 0.1177 0.4141 0.043 Uiso 1 1 calc R . .
C2 C -0.6128(4) 0.2785(3) 0.4241(3) 0.0265(10) Uani 1 1 d . . .
C3 C -0.6147(5) 0.2957(4) 0.3299(3) 0.0279(11) Uani 1 1 d . . .
C4 C -0.5729(4) 0.3913(4) 0.3007(3) 0.0277(11) Uani 1 1 d . . .
C5 C -0.5813(5) 0.4086(4) 0.2035(3) 0.0337(12) Uani 1 1 d . . .
H5A H -0.6152 0.3591 0.1500 0.040 Uiso 1 1 calc R . .
C6 C -0.5317(5) 0.5090(4) 0.2034(4) 0.0357(12) Uani 1 1 d . . .
H6A H -0.5241 0.5438 0.1493 0.043 Uiso 1 1 calc R . .
C7 C -0.4922(5) 0.5541(4) 0.2994(3) 0.0279(11) Uani 1 1 d . . .
C8 C -0.4343(5) 0.6571(4) 0.3273(3) 0.0302(11) Uani 1 1 d . . .
C9 C -0.4063(5) 0.7004(4) 0.4210(3) 0.0301(11) Uani 1 1 d . . .
C10 C -0.3508(5) 0.8063(4) 0.4506(4) 0.0382(13) Uani 1 1 d . . .
H10A H -0.3260 0.8577 0.4107 0.046 Uiso 1 1 calc R . .
C11 C -0.6624(5) 0.2067(4) 0.2554(3) 0.0301(11) Uani 1 1 d . . .
C12 C -0.7938(5) 0.1554(4) 0.2332(4) 0.0416(13) Uani 1 1 d . . .
H12A H -0.8552 0.1778 0.2635 0.050 Uiso 1 1 calc R . .
C13 C -0.8359(5) 0.0703(5) 0.1659(4) 0.0473(15) Uani 1 1 d . . .
C14 C -0.7458(5) 0.0335(4) 0.1255(4) 0.0404(13) Uani 1 1 d . . .
C15 C -0.6134(5) 0.0875(4) 0.1456(3) 0.0313(11) Uani 1 1 d . . .
C16 C -0.5725(5) 0.1746(4) 0.2118(3) 0.0312(11) Uani 1 1 d . . .
H16A H -0.4824 0.2115 0.2266 0.037 Uiso 1 1 calc R . .
C17 C -1.0553(7) 0.0645(8) 0.1574(7) 0.101(3) Uani 1 1 d . . .
H17C H -1.1368 0.0312 0.1161 0.152 Uiso 1 1 calc R . .
H17B H -1.0209 0.1356 0.1475 0.152 Uiso 1 1 calc R . .
H17A H -1.0717 0.0599 0.2234 0.152 Uiso 1 1 calc R . .
C18 C -0.8307(8) -0.1418(5) 0.0894(7) 0.087(3) Uani 1 1 d . . .
H18C H -0.8517 -0.1954 0.0364 0.131 Uiso 1 1 calc R . .
H18B H -0.9092 -0.1465 0.1199 0.131 Uiso 1 1 calc R . .
H18A H -0.7639 -0.1492 0.1352 0.131 Uiso 1 1 calc R . .
C19 C -0.3985(6) 0.1093(5) 0.1090(5) 0.0515(16) Uani 1 1 d . . .
H19C H -0.3538 0.0791 0.0648 0.077 Uiso 1 1 calc R . .
H19B H -0.3612 0.1105 0.1738 0.077 Uiso 1 1 calc R . .
H19A H -0.3879 0.1782 0.0962 0.077 Uiso 1 1 calc R . .
C20 C -0.4097(5) 0.7257(4) 0.2514(4) 0.0330(12) Uani 1 1 d . . .
C21 C -0.4844(6) 0.7862(4) 0.2421(4) 0.0436(14) Uani 1 1 d . . .
H21A H -0.5438 0.7870 0.2867 0.052 Uiso 1 1 calc R . .
C22 C -0.4770(6) 0.8466(4) 0.1697(5) 0.0527(16) Uani 1 1 d . . .
H22A H -0.5280 0.8895 0.1665 0.063 Uiso 1 1 calc R . .
C23 C -0.3954(6) 0.8429(4) 0.1036(4) 0.0475(15) Uani 1 1 d . . .
H23A H -0.3909 0.8831 0.0536 0.057 Uiso 1 1 calc R . .
C24 C -0.3180(5) 0.7812(4) 0.1077(4) 0.0400(14) Uani 1 1 d . . .
C25 C -0.2402(6) 0.7746(5) 0.0352(4) 0.0499(16) Uani 1 1 d . . .
H25A H -0.2403 0.8124 -0.0163 0.060 Uiso 1 1 calc R . .
C26 C -0.1654(7) 0.7150(5) 0.0381(4) 0.0595(19) Uani 1 1 d . . .
H26A H -0.1164 0.7089 -0.0125 0.071 Uiso 1 1 calc R . .
C27 C -0.1601(6) 0.6617(5) 0.1161(4) 0.0490(15) Uani 1 1 d . . .
H27A H -0.1054 0.6215 0.1182 0.059 Uiso 1 1 calc R . .
C28 C -0.2327(5) 0.6670(4) 0.1890(4) 0.0360(12) Uani 1 1 d . . .
C29 C -0.3186(5) 0.7237(4) 0.1853(3) 0.0339(12) Uani 1 1 d . . .
C30 C -0.2026(5) 0.6174(4) 0.2723(4) 0.0385(13) Uani 1 1 d . . .
C31 C 0.0664(7) 0.3005(6) 0.4221(5) 0.067(2) Uani 1 1 d . . .
H31A H 0.1515 0.2953 0.4114 0.101 Uiso 1 1 calc R . .
H31B H 0.0239 0.3117 0.3633 0.101 Uiso 1 1 calc R . .
H31C H 0.0122 0.2379 0.4429 0.101 Uiso 1 1 calc R . .
C32 C -0.2489(7) 0.3356(5) 0.3732(6) 0.074(2) Uani 1 1 d . . .
H32A H -0.2612 0.3018 0.3086 0.110 Uiso 1 1 calc R . .
H32B H -0.3279 0.3501 0.3864 0.110 Uiso 1 1 calc R . .
H32C H -0.2313 0.2916 0.4177 0.110 Uiso 1 1 calc R . .
C33 C 0.2332(7) 0.5723(8) 0.3679(7) 0.101(3) Uani 1 1 d . . .
H33A H 0.2378 0.5892 0.3032 0.152 Uiso 1 1 calc R . .
H33B H 0.2288 0.5021 0.3688 0.152 Uiso 1 1 calc R . .
H33C H 0.3108 0.6167 0.4084 0.152 Uiso 1 1 calc R . .
C34 C 0.0296(15) 0.4084(14) 0.1586(11) 0.150(7) Uani 0.75 1 d P . .
H34A H -0.0044 0.4366 0.2116 0.225 Uiso 0.75 1 calc PR . .
H34B H 0.0612 0.4599 0.1167 0.225 Uiso 0.75 1 calc PR . .
H34C H 0.1013 0.3867 0.1826 0.225 Uiso 0.75 1 calc PR . .
C35 C -0.0298(16) 0.9266(13) 0.3483(15) 0.172(9) Uani 0.75 1 d P . .
H35A H -0.0283 0.9863 0.3894 0.258 Uiso 0.75 1 calc PR . .
H35B H -0.1122 0.9005 0.3067 0.258 Uiso 0.75 1 calc PR . .
H35C H 0.0427 0.9449 0.3100 0.258 Uiso 0.75 1 calc PR . .
C36 C -0.296(3) 1.1304(18) 0.566(2) 0.150(11) Uani 0.50 1 d P . .
C37 C -0.3486(9) 0.3967(7) 0.0248(5) 0.089(3) Uani 1 1 d . . .
H37A H -0.4312 0.4058 0.0371 0.133 Uiso 1 1 calc R . .
H37B H -0.3655 0.3383 -0.0228 0.133 Uiso 1 1 calc R . .
H37C H -0.2926 0.4572 0.0017 0.133 Uiso 1 1 calc R . .
C38 C -0.289(4) 1.086(3) 0.469(3) 0.112(13) Uiso 0.25 1 d P . .
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'
Cu Cu 0.3201 1.2651 '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
N2 Cu1 N2 180.000(1) . 2_466 ?
N2 Cu1 N1 90.36(15) . 2_466 ?
N2 Cu1 N1 89.64(15) 2_466 2_466 ?
N2 Cu1 N1 89.64(15) . . ?
N2 Cu1 N1 90.36(15) 2_466 . ?
N1 Cu1 N1 180.000(1) 2_466 . ?
O7 Mn1 O6 92.61(17) 2_566 2_566 ?
O7 Mn1 O8 88.1(2) 2_566 2_566 ?
O6 Mn1 O8 94.9(2) 2_566 2_566 ?
C13 O3 C17 116.3(5) . . ?
C14 O4 C18 114.5(5) . . ?
C15 O5 C19 117.8(4) . . ?
C4 N1 C7 105.0(4) . . ?
C4 N1 Cu1 127.5(3) . . ?
C7 N1 Cu1 127.3(3) . . ?
C9 N2 C2 105.6(4) . 2_466 ?
C9 N2 Cu1 127.9(3) . . ?
C2 N2 Cu1 126.4(3) 2_466 . ?
C10 C1 C2 106.8(4) 2_466 . ?
N2 C2 C3 126.2(4) 2_466 . ?
N2 C2 C1 110.1(4) 2_466 . ?
C3 C2 C1 123.6(4) . . ?
C2 C3 C4 123.9(4) . . ?
C2 C3 C11 118.3(4) . . ?
C4 C3 C11 117.7(4) . . ?
N1 C4 C3 125.4(4) . . ?
N1 C4 C5 111.1(4) . . ?
C3 C4 C5 123.5(4) . . ?
C6 C5 C4 106.2(4) . . ?
C5 C6 C7 107.8(4) . . ?
N1 C7 C8 125.6(4) . . ?
N1 C7 C6 109.9(4) . . ?
C8 C7 C6 124.4(4) . . ?
C9 C8 C7 123.7(4) . . ?
C9 C8 C20 118.4(4) . . ?
C7 C8 C20 117.8(4) . . ?
N2 C9 C8 125.6(4) . . ?
N2 C9 C10 110.2(4) . . ?
C8 C9 C10 124.2(5) . . ?
C1 C10 C9 107.3(5) 2_466 . ?
C16 C11 C12 120.6(5) . . ?
C16 C11 C3 118.8(4) . . ?
C12 C11 C3 120.6(5) . . ?
C11 C12 C13 119.6(5) . . ?
O3 C13 C12 124.5(6) . . ?
O3 C13 C14 115.2(5) . . ?
C12 C13 C14 120.3(5) . . ?
O4 C14 C15 118.0(5) . . ?
O4 C14 C13 121.7(5) . . ?
C15 C14 C13 119.7(5) . . ?
O5 C15 C14 115.9(4) . . ?
O5 C15 C16 125.0(5) . . ?
C14 C15 C16 119.1(5) . . ?
C11 C16 C15 120.5(5) . . ?
C21 C20 C29 119.7(5) . . ?
C21 C20 C8 118.0(5) . . ?
C29 C20 C8 122.2(5) . . ?
C20 C21 C22 122.7(6) . . ?
C23 C22 C21 118.8(6) . . ?
C22 C23 C24 121.6(5) . . ?
C23 C24 C25 120.2(5) . . ?
C23 C24 C29 120.0(5) . . ?
C25 C24 C29 119.8(6) . . ?
C26 C25 C24 120.7(6) . . ?
C25 C26 C27 120.2(6) . . ?
C28 C27 C26 121.0(6) . . ?
C27 C28 C29 120.2(5) . . ?
C27 C28 C30 114.3(5) . . ?
C29 C28 C30 125.3(5) . . ?
C28 C29 C20 125.2(5) . . ?
C28 C29 C24 117.8(5) . . ?
C20 C29 C24 117.0(5) . . ?
O1 C30 O2 124.4(5) . . ?
O1 C30 C28 118.2(5) . . ?
O2 C30 C28 117.3(5) . . ?
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
Cu1 N2 1.997(4) . ?
Cu1 N2 1.997(4) 2_466 ?
Cu1 N1 1.999(4) 2_466 ?
Cu1 N1 1.999(4) . ?
Mn1 O7 2.136(4) 2_566 ?
Mn1 O6 2.137(4) 2_566 ?
Mn1 O8 2.176(5) 2_566 ?
O1 C30 1.247(7) . ?
O2 C30 1.268(6) . ?
O3 C13 1.361(7) . ?
O3 C17 1.427(10) . ?
O4 C14 1.374(6) . ?
O4 C18 1.408(9) . ?
O5 C15 1.351(6) . ?
O5 C19 1.426(7) . ?
O6 C31 1.423(7) . ?
O7 C32 1.407(7) . ?
O8 C33 1.428(9) . ?
O9 C34 1.295(15) . ?
O10 C35 1.174(17) . ?
O11 C36 1.32(3) . ?
O12 C37 1.391(9) . ?
O13 C38 1.48(5) . ?
N1 C4 1.370(6) . ?
N1 C7 1.384(6) . ?
N2 C9 1.375(6) . ?
N2 C2 1.383(6) 2_466 ?
C1 C10 1.358(7) 2_466 ?
C1 C2 1.435(7) . ?
C2 N2 1.383(6) 2_466 ?
C2 C3 1.393(7) . ?
C3 C4 1.394(7) . ?
C3 C11 1.496(6) . ?
C4 C5 1.438(7) . ?
C5 C6 1.346(7) . ?
C6 C7 1.433(7) . ?
C7 C8 1.392(7) . ?
C8 C9 1.392(7) . ?
C8 C20 1.505(7) . ?
C9 C10 1.430(7) . ?
C10 C1 1.358(7) 2_466 ?
C11 C16 1.379(7) . ?
C11 C12 1.380(7) . ?
C12 C13 1.396(8) . ?
C13 C14 1.396(8) . ?
C14 C15 1.393(7) . ?
C15 C16 1.407(7) . ?
C20 C21 1.370(7) . ?
C20 C29 1.435(7) . ?
C21 C22 1.394(8) . ?
C22 C23 1.362(9) . ?
C23 C24 1.402(8) . ?
C24 C25 1.410(8) . ?
C24 C29 1.436(7) . ?
C25 C26 1.353(10) . ?
C26 C27 1.412(9) . ?
C27 C28 1.375(8) . ?
C28 C29 1.420(8) . ?
C28 C30 1.506(8) . ?
