#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/43/4344381.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_4344381
loop_
_publ_author_name
'Escriche-Tur, Luis'
'Corbella, Montserrat'
'Font-Bardia, Mercè'
'Castro, Isabel'
'Bonneviot, Laurent'
'Albela, Belén'
_publ_section_title
;
 Biomimetic Mn-Catalases Based on Dimeric Manganese Complexes in
 Mesoporous Silica for Potential Antioxidant Agent.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10111
_journal_page_last               10125
_journal_paper_doi               10.1021/acs.inorgchem.5b01425
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'4(C36 H32 Mn2 N5 O11), 4(H2 O), 2(C2 H3 N) , 4(N O3)'
_chemical_formula_sum            'C148 H142 Mn8 N26 O60'
_chemical_formula_weight         3670.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 99.3280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   16.3701(6)
_cell_length_b                   24.5812(9)
_cell_length_c                   9.9600(4)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.39
_cell_volume                     3954.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'high brilliance Incoatec Microfocus Source '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            27952
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1878
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0507
_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)+(0.0799P)²+18.8996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                3363
_reflns_number_total             3515
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic5b01425_si_002.cif
_cod_data_source_block           mo_i14rb75_0m1
_cod_depositor_comments
'Adding full bibliography for 4344381--4344382.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4344381
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
_atom_site_disorder_assembly
_atom_site_disorder_group
N4 N 0.5352(11) 1.0417(5) 0.8748(17) 0.144(6) Uani 0.50 1 d PDU A 1
O9 O 0.5414(12) 1.0394(7) 1.0002(18) 0.172(5) Uani 0.50 1 d PDU A 1
O10 O 0.5437(10) 1.0000(4) 0.8075(19) 0.172(5) Uani 0.50 1 d PDU . 1
O11 O 0.5200(10) 1.0860(4) 0.8219(19) 0.172(5) Uani 0.50 1 d PDU . 1
O2W O 0.5478(12) 1.0582(7) 0.944(2) 0.074(4) Uani 0.25 1 d P B 2
N1W N 0.5057(10) 0.8454(6) 0.9896(13) 0.061(3) Uani 0.25 1 d PDU C 1
C1W C 0.4747(5) 0.8612(3) 0.8770(11) 0.061(3) Uani 0.25 1 d PDU C 1
C2W C 0.4487(12) 0.8919(7) 0.7530(15) 0.061(3) Uani 0.25 1 d PDU . 1
O1W O 0.4747(5) 0.8612(3) 0.8770(11) 0.074(4) Uani 0.25 1 d P D 2
Mn1 Mn 0.44087(3) 0.690595(18) 0.85943(4) 0.01656(19) Uani 1 1 d U . .
N1 N 0.33688(16) 0.73414(11) 0.7765(3) 0.0191(5) Uani 1 1 d U E .
N2 N 0.35329(17) 0.66078(11) 0.9679(3) 0.0216(6) Uani 1 1 d U E .
O1 O 0.5000 0.72488(12) 0.7500 0.0183(6) Uani 1 2 d SU . .
O2 O 0.52701(13) 0.64167(9) 0.9531(2) 0.0217(5) Uani 1 1 d U . .
O3 O 0.39947(13) 0.62646(9) 0.7150(2) 0.0218(5) Uani 1 1 d U E .
O4 O 0.24647(16) 0.59451(13) 0.5827(3) 0.0412(7) Uani 1 1 d U E .
C1 C 0.3359(2) 0.77349(13) 0.6837(3) 0.0227(7) Uani 1 1 d U . .
H1 H 0.3857 0.7846 0.6589 0.027 Uiso 1 1 calc R E .
C2 C 0.2631(2) 0.79816(15) 0.6233(4) 0.0292(8) Uani 1 1 d U E .
H2 H 0.2638 0.8256 0.5592 0.035 Uiso 1 1 calc R . .
C3 C 0.1898(2) 0.78122(18) 0.6600(4) 0.0377(9) Uani 1 1 d U . .
H3 H 0.1400 0.7971 0.6209 0.045 Uiso 1 1 calc R E .
C4 C 0.1906(2) 0.74033(18) 0.7555(4) 0.0388(9) Uani 1 1 d U E .
H4 H 0.1414 0.7282 0.7803 0.047 Uiso 1 1 calc R . .
C5 C 0.2650(2) 0.71777(14) 0.8137(3) 0.0242(7) Uani 1 1 d U . .
C6 C 0.2743(2) 0.67627(14) 0.9220(3) 0.0237(7) Uani 1 1 d U E .
C7 C 0.2084(2) 0.65495(15) 0.9775(4) 0.0305(8) Uani 1 1 d U . .
H7 H 0.1542 0.6651 0.9436 0.037 Uiso 1 1 calc R E .
C8 C 0.2250(2) 0.61838(15) 1.0842(4) 0.0325(8) Uani 1 1 d U E .
H8 H 0.1820 0.6036 1.1228 0.039 Uiso 1 1 calc R . .
C9 C 0.3055(2) 0.60410(14) 1.1324(4) 0.0302(8) Uani 1 1 d U . .
H9 H 0.3176 0.5801 1.2051 0.036 Uiso 1 1 calc R E .
C10 C 0.3683(2) 0.62586(14) 1.0716(3) 0.0259(7) Uani 1 1 d U E .
H10 H 0.4227 0.6159 1.1040 0.031 Uiso 1 1 calc R . .
C11 C 0.41630(19) 0.61744(12) 0.5997(3) 0.0189(6) Uani 1 1 d U . .
C12 C 0.3711(2) 0.57337(13) 0.5139(3) 0.0271(7) Uani 1 1 d U E .
C13 C 0.2880(2) 0.56129(15) 0.5118(4) 0.0360(9) Uani 1 1 d U . .
C14 C 0.2526(3) 0.51606(19) 0.4321(4) 0.0478(11) Uani 1 1 d U E .
H14 H 0.1968 0.5077 0.4268 0.057 Uiso 1 1 calc R . .
C15 C 0.3023(3) 0.48554(17) 0.3643(4) 0.0494(11) Uani 1 1 d U . .
H15 H 0.2789 0.4557 0.3148 0.059 Uiso 1 1 calc R E .
C16 C 0.3840(3) 0.49609(17) 0.3646(4) 0.0477(11) Uani 1 1 d U E .
H16 H 0.4154 0.4736 0.3177 0.057 Uiso 1 1 calc R . .
C17 C 0.4195(3) 0.54058(14) 0.4355(4) 0.0404(10) Uani 1 1 d U . .
H17 H 0.4744 0.5495 0.4328 0.048 Uiso 1 1 calc R E .
C18 C 0.1588(3) 0.5843(3) 0.5792(6) 0.0653(15) Uani 1 1 d U . .
H18A H 0.1366 0.6107 0.6344 0.098 Uiso 1 1 calc R E .
H18B H 0.1513 0.5485 0.6137 0.098 Uiso 1 1 calc R . .
H18C H 0.1305 0.5869 0.4871 0.098 Uiso 1 1 calc R . .
O5 O 0.47192(18) 0.75478(13) 1.0132(3) 0.0431(7) Uani 0.50 1 d PU E 1
N3 N 0.4903(3) 0.7593(2) 1.1304(6) 0.0233(11) Uani 0.50 1 d PU E 1
O7 O 0.4947(3) 0.7162(2) 1.1965(5) 0.0294(11) Uani 0.50 1 d PU . 1
O8 O 0.5009(4) 0.8041(2) 1.1896(5) 0.0373(12) Uani 0.50 1 d PU . 1
O6 O 0.47192(18) 0.75478(13) 1.0132(3) 0.0431(7) Uani 0.50 1 d PU E 2
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'
Mn Mn 0.3368 0.7283 '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'
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
O11 N4 O9 117.1(17) . .
O11 N4 O10 122.4(13) . .
O9 N4 O10 120.5(17) . .
N4 O10 O10 102.1(13) . 2_656
N4 O11 O11 116.6(11) . 2_656
N1W C1W C2W 166.2(11) . .
C1W C2W C2W 82.7(10) . 2_656
O1 Mn1 O2 99.22(9) . .
O1 Mn1 N2 168.48(9) . .
O2 Mn1 N2 92.30(10) . .
O1 Mn1 N1 90.25(9) . .
O2 Mn1 N1 170.36(10) . .
N2 Mn1 N1 78.24(11) . .
O1 Mn1 O3 94.62(9) . .
O2 Mn1 O3 89.60(9) . .
N2 Mn1 O3 85.41(10) . .
N1 Mn1 O3 87.86(9) . .
O1 Mn1 O5 89.98(11) . .
O2 Mn1 O5 92.37(10) . .
N2 Mn1 O5 89.54(11) . .
N1 Mn1 O5 89.39(11) . .
O3 Mn1 O5 174.65(10) . .
O1 Mn1 Mn1 28.22(8) . 2_656
O2 Mn1 Mn1 81.62(7) . 2_656
N2 Mn1 Mn1 157.15(8) . 2_656
N1 Mn1 Mn1 106.43(7) . 2_656
O3 Mn1 Mn1 72.61(6) . 2_656
O5 Mn1 Mn1 112.60(8) . 2_656
C1 N1 C5 119.5(3) . .
C1 N1 Mn1 124.6(2) . .
C5 N1 Mn1 115.7(2) . .
C10 N2 C6 119.2(3) . .
C10 N2 Mn1 125.2(2) . .
C6 N2 Mn1 115.5(2) . .
Mn1 O1 Mn1 123.56(17) . 2_656
C11 O2 Mn1 126.8(2) 2_656 .
C11 O3 Mn1 130.6(2) . .
C13 O4 C18 117.9(4) . .
N1 C1 C2 122.0(3) . .
N1 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
C3 C2 C1 118.6(3) . .
C3 C2 H2 120.7 . .
C1 C2 H2 120.7 . .
C2 C3 C4 119.4(3) . .
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C5 C4 C3 119.4(3) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
N1 C5 C4 121.0(3) . .
N1 C5 C6 114.6(3) . .
C4 C5 C6 124.4(3) . .
N2 C6 C7 121.3(3) . .
N2 C6 C5 114.8(3) . .
C7 C6 C5 123.8(3) . .
C8 C7 C6 118.7(3) . .
C8 C7 H7 120.6 . .
C6 C7 H7 120.6 . .
C9 C8 C7 119.5(3) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C8 C9 C10 119.2(3) . .
C8 C9 H9 120.4 . .
C10 C9 H9 120.4 . .
N2 C10 C9 122.1(3) . .
N2 C10 H10 119.0 . .
C9 C10 H10 119.0 . .
O3 C11 O2 125.3(3) . 2_656
O3 C11 C12 119.5(3) . .
O2 C11 C12 115.1(3) 2_656 .
C13 C12 C17 119.6(3) . .
C13 C12 C11 123.7(3) . .
C17 C12 C11 116.6(3) . .
O4 C13 C12 116.3(3) . .
O4 C13 C14 125.0(4) . .
C12 C13 C14 118.7(4) . .
C15 C14 C13 118.8(4) . .
C15 C14 H14 120.6 . .
C13 C14 H14 120.6 . .
C16 C15 C14 123.9(4) . .
C16 C15 H15 118.0 . .
C14 C15 H15 118.0 . .
C15 C16 C17 119.0(5) . .
C15 C16 H16 120.5 . .
C17 C16 H16 120.5 . .
C16 C17 C12 119.8(4) . .
C16 C17 H17 120.1 . .
C12 C17 H17 120.1 . .
O4 C18 H18A 109.5 . .
O4 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
O4 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N3 O5 Mn1 139.5(4) . .
O5 N3 O7 115.7(5) . .
O5 N3 O8 123.5(6) . .
O7 N3 O8 120.7(5) . .
O7 O7 N3 121.5(3) 2_657 .
O8 O8 N3 116.5(4) 2_657 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N4 O11 1.217(9) .
N4 O9 1.238(10) .
N4 O10 1.246(9) .
O10 O10 1.68(3) 2_656
O11 O11 1.48(3) 2_656
N1W C1W 1.218(3) .
C1W C2W 1.4508(10) .
C2W C2W 1.69(4) 2_656
Mn1 O1 1.7824(14) .
Mn1 O2 1.970(2) .
Mn1 N2 2.064(3) .
Mn1 N1 2.067(3) .
Mn1 O3 2.167(2) .
Mn1 O5 2.200(3) .
Mn1 Mn1 3.1412(9) 2_656
N1 C1 1.336(4) .
N1 C5 1.351(4) .
N2 C10 1.335(4) .
N2 C6 1.355(4) .
O1 Mn1 1.7824(14) 2_656
O2 C11 1.285(4) 2_656
O3 C11 1.244(4) .
O4 C13 1.335(5) .
O4 C18 1.453(5) .
C1 C2 1.385(5) .
C1 H1 0.9300 .
C2 C3 1.375(5) .
C2 H2 0.9300 .
C3 C4 1.383(5) .
C3 H3 0.9300 .
C4 C5 1.378(5) .
C4 H4 0.9300 .
C5 C6 1.475(5) .
C6 C7 1.391(5) .
C7 C8 1.385(5) .
C7 H7 0.9300 .
C8 C9 1.373(6) .
C8 H8 0.9300 .
C9 C10 1.382(5) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 O2 1.285(4) 2_656
C11 C12 1.499(4) .
C12 C13 1.389(5) .
C12 C17 1.445(6) .
C13 C14 1.433(6) .
C14 C15 1.363(7) .
C14 H14 0.9300 .
C15 C16 1.363(7) .
C15 H15 0.9300 .
C16 C17 1.378(5) .
C16 H16 0.9300 .
C17 H17 0.9300 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
O5 N3 1.162(6) .
N3 O7 1.243(8) .
N3 O8 1.247(8) .
O7 O7 1.052(9) 2_657
O8 O8 1.209(11) 2_657
