#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:30:31 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179582 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/47/4504784.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_4504784
loop_
_publ_author_name
'George, Sumod'
'Goldberg, Israel'
_publ_section_title
;
 Self-Assembly of Supramolecular Porphyrin Arrays by Hydrogen
 Bonding:  New Structures and Reflections
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              755
_journal_paper_doi               10.1021/cg050624m
_journal_volume                  6
_journal_year                    2006
_chemical_formula_moiety         'C50 H36 Mn N4 O10, H2 P O4'
_chemical_formula_sum            'C50 H38 Mn N4 O14 P'
_chemical_formula_weight         1004.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6724(6)
_cell_length_b                   18.6724(6)
_cell_length_c                   16.8341(5)
_cell_measurement_reflns_used    6927
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.44
_cell_volume                     5869.4(3)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '0.7 deg. Phi 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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11027
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.44
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0663
_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)+(0.1149P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                3964
_reflns_number_total             5680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050624msi20051123_105943.cif
_cod_data_source_block           Compound-3
_cod_original_sg_symbol_H-M      'P 43212'
_cod_database_code               4504784
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+1/4'
'-y+1/2, x+1/2, z+3/4'
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
Mn Mn 0.11464(3) 0.11464(3) 0.0000 0.0314(2) Uani 1 2 d S
C1 C 0.0541(2) -0.0381(2) 0.0090(3) 0.0362(10) Uani 1 1 d .
C2 C 0.0777(2) -0.1107(2) 0.0205(3) 0.0428(11) Uani 1 1 d .
H2 H 0.0480 -0.1521 0.0209 0.051 Uiso 1 1 calc R
C3 C 0.1482(3) -0.1098(2) 0.0306(3) 0.0426(11) Uani 1 1 d .
H3 H 0.1778 -0.1503 0.0396 0.051 Uiso 1 1 calc R
C4 C 0.1718(2) -0.0362(2) 0.0255(3) 0.0366(10) Uani 1 1 d .
C5 C 0.2413(2) -0.0136(2) 0.0376(3) 0.0398(10) Uani 1 1 d .
C6 C 0.2636(2) 0.0574(2) 0.0319(3) 0.0393(11) Uani 1 1 d .
C7 C 0.3372(2) 0.0804(2) 0.0408(3) 0.0463(12) Uani 1 1 d .
H7 H 0.3772 0.0509 0.0529 0.056 Uiso 1 1 calc R
C8 C 0.3379(2) 0.1525(2) 0.0285(3) 0.0426(11) Uani 1 1 d .
H8 H 0.3791 0.1824 0.0283 0.051 Uiso 1 1 calc R
C9 C 0.2664(2) 0.1750(2) 0.0159(3) 0.0376(10) Uani 1 1 d .
C10 C 0.2458(2) 0.2458(2) 0.0000 0.0353(13) Uani 1 2 d S
C11 C -0.0160(2) -0.0160(2) 0.0000 0.0394(15) Uani 1 2 d S
N12 N 0.1133(2) 0.00751(17) 0.0129(2) 0.0360(8) Uani 1 1 d .
N13 N 0.22110(16) 0.11630(18) 0.0183(2) 0.0338(8) Uani 1 1 d .
C14 C -0.0734(2) -0.0734(2) 0.0000 0.0478(17) Uani 1 2 d S
C15 C -0.0819(3) -0.1170(3) -0.0643(4) 0.0675(17) Uani 1 1 d .
H15 H -0.0521 -0.1109 -0.1095 0.081 Uiso 1 1 calc R
C16 C -0.1338(3) -0.1702(3) -0.0641(4) 0.0712(18) Uani 1 1 d .
H16 H -0.1384 -0.2010 -0.1087 0.085 Uiso 1 1 calc R
C17 C -0.1787(2) -0.1787(2) 0.0000 0.0477(16) Uani 1 2 d S
C18 C -0.2344(2) -0.2344(2) 0.0000 0.0521(18) Uani 1 2 d S
O19 O -0.2378(2) -0.2754(2) -0.0603(2) 0.0658(11) Uani 1 1 d .
H19 H -0.2745 -0.3078 -0.0535 0.079 Uiso 0.50 1 calc PR
C20 C 0.3019(2) 0.3019(2) 0.0000 0.0353(14) Uani 1 2 d S
C21 C 0.3423(2) 0.3152(2) 0.0679(3) 0.0443(11) Uani 1 1 d .
H21 H 0.3334 0.2887 0.1151 0.053 Uiso 1 1 calc R
C22 C 0.3958(2) 0.3672(2) 0.0673(3) 0.0416(10) Uani 1 1 d .
H22 H 0.4242 0.3747 0.1134 0.050 Uiso 1 1 calc R
C23 C 0.4077(2) 0.4077(2) 0.0000 0.0347(14) Uani 1 2 d S
C24 C 0.4646(2) 0.4646(2) 0.0000 0.0312(12) Uani 1 2 d S
O25 O 0.50834(16) 0.46587(16) 0.0569(2) 0.0450(8) Uani 1 1 d .
H25 H 0.5401 0.5030 0.0498 0.054 Uiso 0.50 1 calc PR
C26 C 0.2971(2) -0.0691(2) 0.0561(3) 0.0454(11) Uani 1 1 d .
C27 C 0.3123(3) -0.0856(3) 0.1336(3) 0.0555(13) Uani 1 1 d .
H27 H 0.2861 -0.0636 0.1753 0.067 Uiso 1 1 calc R
C28 C 0.3663(3) -0.1350(3) 0.1512(3) 0.0612(14) Uani 1 1 d .
H28 H 0.3774 -0.1458 0.2049 0.073 Uiso 1 1 calc R
C29 C 0.4032(3) -0.1679(3) 0.0910(3) 0.0488(12) Uani 1 1 d .
C30 C 0.3886(3) -0.1542(3) 0.0129(3) 0.0608(14) Uani 1 1 d .
H30 H 0.4134 -0.1787 -0.0282 0.073 Uiso 1 1 calc R
C31 C 0.3343(3) -0.1014(3) -0.0055(3) 0.0554(13) Uani 1 1 d .
H31 H 0.3243 -0.0890 -0.0591 0.066 Uiso 1 1 calc R
C32 C 0.4623(3) -0.2196(3) 0.1121(4) 0.0537(13) Uani 1 1 d .
O33 O 0.4813(2) -0.2329(2) 0.1777(3) 0.0705(12) Uani 1 1 d .
O34 O 0.4917(2) -0.2482(2) 0.0491(3) 0.0740(12) Uani 1 1 d .
H34 H 0.5275 -0.2791 0.0644 0.089 Uiso 1 1 calc R
O35 O 0.13520(16) 0.09555(17) -0.12920(17) 0.0431(7) Uani 1 1 d .
H35 H 0.1011 0.0661 -0.1509 0.052 Uiso 1 1 d R
C36 C 0.1476(4) 0.1476(4) -0.1865(4) 0.091(2) Uani 1 1 d .
H36A H 0.1026 0.1590 -0.2137 0.137 Uiso 1 1 calc R
H36B H 0.1824 0.1297 -0.2252 0.137 Uiso 1 1 calc R
H36C H 0.1665 0.1909 -0.1611 0.137 Uiso 1 1 calc R
P37 P 0.38515(6) 0.38515(6) 0.5000 0.0383(3) Uani 1 2 d S
O38 O 0.31886(14) 0.38448(17) 0.44654(18) 0.0405(7) Uani 1 1 d .
O39 O 0.38249(18) 0.45613(15) 0.54724(19) 0.0444(8) 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'
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'
P P 0.1023 0.0942 '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'
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
N13 Mn N13 89.6(2) 6 .
N13 Mn N12 90.66(14) 6 6
N13 Mn N12 177.36(15) . 6
N13 Mn N12 177.36(15) 6 .
N13 Mn N12 90.65(14) . .
N12 Mn N12 89.2(2) 6 .
N13 Mn O35 88.96(12) 6 6
N13 Mn O35 90.32(13) . 6
N12 Mn O35 87.05(13) 6 6
N12 Mn O35 93.66(13) . 6
N13 Mn O35 90.33(13) 6 .
N13 Mn O35 88.96(12) . .
N12 Mn O35 93.67(13) 6 .
N12 Mn O35 87.05(13) . .
O35 Mn O35 179.00(17) 6 .
N12 C1 C11 124.9(4) . .
N12 C1 C2 109.1(4) . .
C11 C1 C2 125.9(4) . .
C3 C2 C1 108.0(4) . .
C3 C2 H2 126.0 . .
C1 C2 H2 126.0 . .
C2 C3 C4 107.9(4) . .
C2 C3 H3 126.0 . .
C4 C3 H3 126.0 . .
N12 C4 C5 125.9(4) . .
N12 C4 C3 109.2(4) . .
C5 C4 C3 124.7(4) . .
C4 C5 C6 124.2(4) . .
C4 C5 C26 118.2(4) . .
C6 C5 C26 117.6(4) . .
N13 C6 C5 126.8(4) . .
N13 C6 C7 109.1(4) . .
C5 C6 C7 124.1(4) . .
C8 C7 C6 106.7(4) . .
C8 C7 H7 126.6 . .
C6 C7 H7 126.6 . .
C7 C8 C9 107.8(4) . .
C7 C8 H8 126.1 . .
C9 C8 H8 126.1 . .
N13 C9 C10 125.8(4) . .
N13 C9 C8 109.7(4) . .
C10 C9 C8 124.5(4) . .
C9 C10 C9 123.6(5) 6 .
C9 C10 C20 118.2(3) 6 .
C9 C10 C20 118.2(3) . .
C1 C11 C1 125.3(5) 6 .
C1 C11 C14 117.3(3) 6 .
C1 C11 C14 117.3(3) . .
C4 N12 C1 105.8(3) . .
C4 N12 Mn 126.5(3) . .
C1 N12 Mn 127.7(3) . .
C6 N13 C9 106.6(3) . .
C6 N13 Mn 125.7(3) . .
C9 N13 Mn 127.7(3) . .
C15 C14 C15 119.6(6) . 6
C15 C14 C11 120.2(3) . .
C15 C14 C11 120.2(3) 6 .
C14 C15 C16 120.4(5) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C17 C16 C15 120.7(5) . .
C17 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
C16 C17 C16 118.3(6) . 6
C16 C17 C18 120.9(3) . .
C16 C17 C18 120.9(3) 6 .
O19 C18 O19 125.1(6) 6 .
O19 C18 C17 117.5(3) 6 .
O19 C18 C17 117.5(3) . .
C18 O19 H19 109.5 . .
C21 C20 C21 118.7(5) 6 .
C21 C20 C10 120.7(3) 6 .
C21 C20 C10 120.7(3) . .
C22 C21 C20 120.5(4) . .
C22 C21 H21 119.8 . .
C20 C21 H21 119.8 . .
C23 C22 C21 120.3(4) . .
C23 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
C22 C23 C22 119.7(5) 6 .
C22 C23 C24 120.2(3) 6 .
C22 C23 C24 120.2(3) . .
O25 C24 O25 123.7(5) 6 .
O25 C24 C23 118.2(3) 6 .
O25 C24 C23 118.2(3) . .
C24 O25 H25 109.5 . .
C27 C26 C31 120.7(4) . .
C27 C26 C5 119.7(4) . .
C31 C26 C5 119.6(5) . .
C26 C27 C28 120.0(5) . .
C26 C27 H27 120.0 . .
C28 C27 H27 120.0 . .
C29 C28 C27 120.1(5) . .
C29 C28 H28 120.0 . .
C27 C28 H28 120.0 . .
C30 C29 C28 121.8(5) . .
C30 C29 C32 119.4(5) . .
C28 C29 C32 118.7(5) . .
C29 C30 C31 118.2(5) . .
C29 C30 H30 120.9 . .
C31 C30 H30 120.9 . .
C26 C31 C30 119.2(5) . .
C26 C31 H31 120.4 . .
C30 C31 H31 120.4 . .
O33 C32 O34 123.0(5) . .
O33 C32 C29 124.8(5) . .
O34 C32 C29 112.2(5) . .
C32 O34 H34 109.5 . .
C36 O35 Mn 126.3(4) . .
C36 O35 H35 105.0 . .
Mn O35 H35 111.3 . .
O35 C36 H36A 109.5 . .
O35 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
O35 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
O38 P37 O38 109.4(3) . 6_556
O38 P37 O39 106.47(18) . .
O38 P37 O39 112.99(16) 6_556 .
O38 P37 O39 112.99(16) . 6_556
O38 P37 O39 106.47(18) 6_556 6_556
O39 P37 O39 108.6(3) . 6_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn N13 2.012(3) 6
Mn N13 2.012(3) .
Mn N12 2.012(3) 6
Mn N12 2.012(3) .
Mn O35 2.237(3) 6
Mn O35 2.237(3) .
C1 N12 1.397(5) .
C1 C11 1.381(5) .
C1 C2 1.438(6) .
C2 C3 1.327(6) .
C2 H2 0.9500 .
C3 C4 1.446(6) .
C3 H3 0.9500 .
C4 N12 1.381(6) .
C4 C5 1.379(6) .
C5 C6 1.393(6) .
C5 C26 1.502(6) .
C6 N13 1.376(5) .
C6 C7 1.447(6) .
C7 C8 1.362(6) .
C7 H7 0.9500 .
C8 C9 1.416(6) .
C8 H8 0.9500 .
C9 N13 1.385(5) .
C9 C10 1.402(5) .
C10 C9 1.402(5) 6
C10 C20 1.480(8) .
C11 C1 1.381(5) 6
C11 C14 1.516(8) .
C14 C15 1.363(6) .
C14 C15 1.363(6) 6
C15 C16 1.389(7) .
C15 H15 0.9500 .
C16 C17 1.376(7) .
C16 H16 0.9500 .
C17 C16 1.376(7) 6
C17 C18 1.470(9) .
C18 O19 1.274(5) 6
C18 O19 1.274(5) .
O19 H19 0.9200 .
C20 C21 1.393(6) 6
C20 C21 1.393(6) .
C21 C22 1.391(6) .
C21 H21 0.9500 .
C22 C23 1.381(5) .
C22 H22 0.9500 .
C23 C22 1.381(5) 6
C23 C24 1.501(8) .
C24 O25 1.259(4) 6
C24 O25 1.259(4) .
O25 H25 0.9200 .
C26 C27 1.371(7) .
C26 C31 1.386(7) .
C27 C28 1.398(7) .
C27 H27 0.9500 .
C28 C29 1.370(7) .
C28 H28 0.9500 .
C29 C30 1.367(8) .
C29 C32 1.509(7) .
C30 C31 1.448(7) .
C30 H30 0.9500 .
C31 H31 0.9500 .
C32 O33 1.187(7) .
C32 O34 1.308(7) .
O34 H34 0.9200 .
O35 C36 1.389(7) .
O35 H35 0.9174 .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
P37 O38 1.531(3) .
P37 O38 1.531(3) 6_556
P37 O39 1.546(3) .
P37 O39 1.546(3) 6_556
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
O19 H19 O38 0.92 1.65 2.539(4) 160.2 2_554
O25 H25 O39 0.92 1.64 2.511(4) 157.6 2_664
O34 H34 O38 0.92 1.81 2.663(5) 152.5 5_655
O35 H35 O25 0.92 1.80 2.715(4) 179.9 8_544
