#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/24/7002483.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_7002483
loop_
_publ_author_name
'Banu, Kazi Sabnam'
'Chattopadhyay, Tanmay'
'Banerjee, Arpita'
'Mukherjee, Madhuparna'
'Bhattacharya, Santanu'
'Patra, Goutam Kumar'
'Zangrando, Ennio'
'Das, Debasis'
_publ_section_title
;
 Mono- and dinuclear manganese(III) complexes showing efficient
 catechol oxidase activity: syntheses, characterization and
 spectroscopic studies
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8755
_journal_page_last               8764
_journal_paper_doi               10.1039/b902498k
_journal_year                    2009
_chemical_formula_moiety
'2(C21 H24 Mn N2 O6, 2(Cl), 4(H2 O), (C2 H3 N)'
_chemical_formula_sum            'C44 H59 Cl2 Mn2 N5 O16'
_chemical_formula_weight         1094.74
_chemical_name_systematic
;
?
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :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                   26.701(5)
_cell_length_b                   19.466(4)
_cell_length_c                   10.047(3)
_cell_measurement_temperature    293(2)
_cell_volume                     5222(2)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Xpress'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.70.00 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'image plate dip1030'
_diffrn_measurement_method       'laser scanner'
_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  0.0795
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            28162
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2206
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0480
_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)+(0.0836P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                1104
_reflns_number_total             2206
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b902498k.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C cca'
_cod_original_formula_sum        'C44 H59 Cl2 Mn2 N5 O16 '
_cod_database_code               7002483
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'x+1/2, -y, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z'
'x+1, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x-1/2, y, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z'
'-x, y+1/2, z-1/2'
'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
Mn Mn 0.12998(3) 0.2500 0.7500 0.0672(3) Uani 1 2 d S . .
O1W O 0.13314(12) 0.32555(18) 0.5811(4) 0.0999(11) Uani 1 1 d D . .
H2W H 0.1040(12) 0.335(3) 0.554(6) 0.150 Uiso 1 1 d D . .
H1W H 0.1591(15) 0.350(2) 0.590(6) 0.150 Uiso 1 1 d D . .
N1 N 0.18581(13) 0.2002(2) 0.6643(4) 0.0803(11) Uani 1 1 d D . .
O1 O 0.08115(10) 0.19947(14) 0.6584(3) 0.0751(8) Uani 1 1 d . . .
C1 C 0.18133(18) 0.1558(3) 0.5710(5) 0.0808(13) Uani 1 1 d . . .
H1 H 0.2106 0.1372 0.5363 0.097 Uiso 1 1 calc R . .
C2 C 0.13502(18) 0.1325(2) 0.5161(4) 0.0701(12) Uani 1 1 d . . .
C3 C 0.1370(2) 0.0844(2) 0.4123(5) 0.0835(14) Uani 1 1 d . . .
H3 H 0.1683 0.0709 0.3816 0.100 Uiso 1 1 calc R . .
C4 C 0.0952(2) 0.0557(2) 0.3528(5) 0.0845(14) Uani 1 1 d . . .
C5 C 0.04952(19) 0.0767(2) 0.4017(5) 0.0819(13) Uani 1 1 d . . .
H5 H 0.0207 0.0579 0.3648 0.098 Uiso 1 1 calc R . .
C6 C 0.04436(17) 0.1244(2) 0.5035(4) 0.0671(11) Uani 1 1 d . . .
C7 C 0.08713(17) 0.15358(19) 0.5614(4) 0.0658(11) Uani 1 1 d . . .
C8 C 0.0992(2) 0.0041(3) 0.2405(5) 0.1171(19) Uani 1 1 d . . .
H8A H 0.0953 -0.0415 0.2754 0.176 Uiso 1 1 calc R . .
H8B H 0.1314 0.0082 0.1988 0.176 Uiso 1 1 calc R . .
H8C H 0.0734 0.0130 0.1761 0.176 Uiso 1 1 calc R . .
C9 C -0.0052(2) 0.1447(2) 0.5472(5) 0.0842(14) Uani 1 1 d . . .
H9 H -0.0075 0.1781 0.6131 0.101 Uiso 1 1 calc R . .
O2 O -0.04377(15) 0.1211(2) 0.5039(4) 0.1217(14) Uani 1 1 d . . .
C10A C 0.2349(3) 0.2114(4) 0.7457(11) 0.095(2) Uiso 0.50 1 d PD . 1
H10A H 0.2336 0.1895 0.8335 0.114 Uiso 0.50 1 calc PR . 1
C11 C 0.2822(3) 0.1979(4) 0.6762(9) 0.086(3) Uani 0.50 1 d PD . 1
H11A H 0.2861 0.1493 0.6635 0.129 Uiso 0.50 1 calc PR . 1
H11B H 0.3096 0.2150 0.7284 0.129 Uiso 0.50 1 calc PR . 1
H11C H 0.2819 0.2204 0.5912 0.129 Uiso 0.50 1 calc PR . 1
C10B C 0.2346(3) 0.2304(5) 0.6893(9) 0.095(2) Uiso 0.50 1 d PD . 2
H10D H 0.2595 0.1943 0.6952 0.114 Uiso 0.50 1 calc PR . 2
H10E H 0.2436 0.2602 0.6155 0.114 Uiso 0.50 1 calc PR . 2
O2W O 0.20871(14) 0.41890(16) 0.5663(3) 0.0937(10) Uani 1 1 d D . .
H3W H 0.217(2) 0.443(3) 0.499(4) 0.140 Uiso 1 1 d D . .
H4W H 0.214(2) 0.445(2) 0.633(4) 0.140 Uiso 1 1 d D . .
Cl1 Cl 0.2500 0.0000 0.68393(17) 0.0901(6) Uani 1 2 d S . .
N20 N -0.0179(10) 0.2500 0.2500 0.186(4) Uiso 0.50 2 d SPD . .
C20 C 0.0259(11) 0.2500 0.2500 0.186(4) Uiso 0.50 2 d SPD . .
C21 C 0.0826(7) 0.2500 0.2500 0.158(7) Uiso 0.50 2 d SPD . .
H21A H 0.0863 0.2035 0.2500 0.236 Uiso 0.25 1 d PR . .
H21B H 0.0863 0.2733 0.3280 0.236 Uiso 0.25 1 d PR . .
H21C H 0.0863 0.2733 0.1720 0.236 Uiso 0.25 1 d PR . .
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'
Cl Cl 0.1484 0.1585 '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'
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
O1 Mn O1 91.89(17) . 7_456 ?
O1 Mn N1 174.96(15) . 7_456 ?
O1 Mn N1 93.06(14) 7_456 7_456 ?
O1 Mn N1 93.06(14) . . ?
O1 Mn N1 174.96(15) 7_456 . ?
N1 Mn N1 82.0(2) 7_456 . ?
O1 Mn O1W 93.07(13) . 7_456 ?
O1 Mn O1W 89.92(13) 7_456 7_456 ?
N1 Mn O1W 87.91(14) 7_456 7_456 ?
N1 Mn O1W 88.84(14) . 7_456 ?
O1 Mn O1W 89.92(13) . . ?
O1 Mn O1W 93.07(13) 7_456 . ?
N1 Mn O1W 88.84(14) 7_456 . ?
N1 Mn O1W 87.91(14) . . ?
O1W Mn O1W 175.69(16) 7_456 . ?
C1 N1 C10B 119.0(5) . . ?
C1 N1 C10A 123.8(5) . . ?
C10B N1 C10A 25.7(6) . . ?
C1 N1 Mn 125.4(3) . . ?
C10B N1 Mn 113.8(4) . . ?
C10A N1 Mn 109.7(4) . . ?
C7 O1 Mn 128.9(3) . . ?
N1 C1 C2 125.3(4) . . ?
C3 C2 C7 117.7(5) . . ?
C3 C2 C1 117.8(4) . . ?
C7 C2 C1 124.4(4) . . ?
C4 C3 C2 124.1(4) . . ?
C5 C4 C3 116.1(4) . . ?
C5 C4 C8 121.6(5) . . ?
C3 C4 C8 122.2(5) . . ?
C4 C5 C6 123.3(5) . . ?
C5 C6 C7 119.7(4) . . ?
C5 C6 C9 119.8(4) . . ?
C7 C6 C9 120.5(4) . . ?
O1 C7 C6 118.5(4) . . ?
O1 C7 C2 122.5(4) . . ?
C6 C7 C2 119.0(4) . . ?
O2 C9 C6 124.4(4) . . ?
C11 C10A C10A 101.9(6) . 7_456 ?
C11 C10A N1 116.7(8) . . ?
C10A C10A N1 99.7(6) 7_456 . ?
C10B C10B N1 111.2(5) 7_456 . ?
N20 C20 C21 180.000(1) . . ?
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
Mn O1 1.875(3) . ?
Mn O1 1.875(3) 7_456 ?
Mn N1 1.976(4) 7_456 ?
Mn N1 1.976(4) . ?
Mn O1W 2.247(3) 7_456 ?
Mn O1W 2.247(3) . ?
N1 C1 1.281(6) . ?
N1 C10B 1.452(8) . ?
N1 C10A 1.560(9) . ?
O1 C7 1.332(4) . ?
C1 C2 1.428(6) . ?
C2 C3 1.403(6) . ?
C2 C7 1.418(6) . ?
C3 C4 1.383(6) . ?
C4 C5 1.377(6) . ?
C4 C8 1.514(6) . ?
C5 C6 1.388(6) . ?
C6 C7 1.402(6) . ?
C6 C9 1.449(6) . ?
C9 O2 1.208(5) . ?
C10A C11 1.468(10) . ?
C10A C10A 1.506(14) 7_456 ?
C10B C10B 1.438(14) 7_456 ?
N20 C20 1.170(15) . ?
C20 C21 1.51(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Mn N1 C1 5.9(4) . . . . ?
O1 Mn N1 C1 174.7(14) 7_456 . . . ?
N1 Mn N1 C1 -173.1(5) 7_456 . . . ?
O1W Mn N1 C1 98.9(4) 7_456 . . . ?
O1W Mn N1 C1 -83.9(4) . . . . ?
O1 Mn N1 C10B 170.1(5) . . . . ?
O1 Mn N1 C10B -21.0(17) 7_456 . . . ?
N1 Mn N1 C10B -8.8(5) 7_456 . . . ?
O1W Mn N1 C10B -96.9(5) 7_456 . . . ?
O1W Mn N1 C10B 80.3(5) . . . . ?
O1 Mn N1 C10A -162.5(4) . . . . ?
O1 Mn N1 C10A 6.3(17) 7_456 . . . ?
N1 Mn N1 C10A 18.5(4) 7_456 . . . ?
O1W Mn N1 C10A -69.5(4) 7_456 . . . ?
O1W Mn N1 C10A 107.7(4) . . . . ?
O1 Mn O1 C7 174.4(4) 7_456 . . . ?
N1 Mn O1 C7 5.5(17) 7_456 . . . ?
N1 Mn O1 C7 -6.6(3) . . . . ?
O1W Mn O1 C7 -95.6(3) 7_456 . . . ?
O1W Mn O1 C7 81.3(3) . . . . ?
C10B N1 C1 C2 -166.0(6) . . . . ?
C10A N1 C1 C2 164.3(5) . . . . ?
Mn N1 C1 C2 -2.5(6) . . . . ?
N1 C1 C2 C3 178.9(4) . . . . ?
N1 C1 C2 C7 -2.7(7) . . . . ?
C7 C2 C3 C4 -0.8(6) . . . . ?
C1 C2 C3 C4 177.7(4) . . . . ?
C2 C3 C4 C5 -0.4(7) . . . . ?
C2 C3 C4 C8 179.7(4) . . . . ?
C3 C4 C5 C6 0.9(7) . . . . ?
C8 C4 C5 C6 -179.2(4) . . . . ?
C4 C5 C6 C7 -0.1(6) . . . . ?
C4 C5 C6 C9 178.7(4) . . . . ?
Mn O1 C7 C6 -177.1(3) . . . . ?
Mn O1 C7 C2 3.8(5) . . . . ?
C5 C6 C7 O1 179.7(3) . . . . ?
C9 C6 C7 O1 0.9(6) . . . . ?
C5 C6 C7 C2 -1.2(6) . . . . ?
C9 C6 C7 C2 -180.0(4) . . . . ?
C3 C2 C7 O1 -179.4(3) . . . . ?
C1 C2 C7 O1 2.2(6) . . . . ?
C3 C2 C7 C6 1.6(5) . . . . ?
C1 C2 C7 C6 -176.9(4) . . . . ?
C5 C6 C9 O2 2.5(8) . . . . ?
C7 C6 C9 O2 -178.7(5) . . . . ?
C1 N1 C10A C11 30.7(9) . . . . ?
C10B N1 C10A C11 -56.6(11) . . . . ?
Mn N1 C10A C11 -160.7(6) . . . . ?
C1 N1 C10A C10A 139.4(7) . . . 7_456 ?
C10B N1 C10A C10A 52.1(9) . . . 7_456 ?
Mn N1 C10A C10A -52.0(9) . . . 7_456 ?
C1 N1 C10B C10B -169.9(9) . . . 7_456 ?
C10A N1 C10B C10B -61.5(11) . . . 7_456 ?
Mn N1 C10B C10B 24.7(13) . . . 7_456 ?
