#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:27:03 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180435 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/04/7210401.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_7210401
loop_
_publ_author_name
'Khullar, Sadhika'
'Mandal, Sanjay K.'
_publ_section_title
;
 Structural diversity of the encapsulated water clusters in the 3D
 supramolecular assemblies: a cyclic quasi-planar hexamer of water
 constructed through strong hydrogen bonding interactions
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              6652
_journal_paper_doi               10.1039/c3ce40882e
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C44 H40 N8 Mn2 O8, 8(H2O)'
_chemical_formula_sum            'C44 H56 Mn2 N8 O16'
_chemical_formula_weight         1062.85
_chemical_name_common            '[Mn2(tpa)2(fumarate)2].8H2O'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
_cell_angle_alpha                90
_cell_angle_beta                 106.014(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.877(5)
_cell_length_b                   14.366(3)
_cell_length_c                   16.576(4)
_cell_measurement_reflns_used    107
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      23.5979
_cell_measurement_theta_min      4.7163
_cell_volume                     4778.5(19)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 V2011.4-1 (Bruker AXS)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS)'
_computing_publication_material  'SHELXTL (Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX 2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16298
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.74
_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'block shaped'
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.560
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0445
_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)+(0.0523P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                3037
_reflns_number_total             4199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40882e.txt
_cod_data_source_block           2
_cod_database_code               7210401
loop_
_space_group_symop_operation_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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Mn Mn1 0.24158(2) 0.46622(4) 0.38410(3) 0.01731(16) Uani d . 1
N N2 0.17183(13) 0.56645(19) 0.28578(15) 0.0217(7) Uani d . 1
N N4 0.16054(14) 0.37509(19) 0.29721(15) 0.0218(7) Uani d . 1
N N1 0.28883(13) 0.47105(19) 0.27786(14) 0.0203(6) Uani d . 1
N N3 0.28381(13) 0.61123(19) 0.41497(15) 0.0201(6) Uani d . 1
O O1 0.17508(11) 0.48324(15) 0.46029(12) 0.0220(5) Uani d . 1
O O4 0.07671(13) 0.44727(18) 0.47835(16) 0.0400(7) Uani d . 1
O O3 0.09949(12) 0.09614(17) 0.49903(13) 0.0286(6) Uani d . 1
O O5 0.01150(13) 0.61194(17) 0.43536(15) 0.0311(6) Uani d G 1
H H5A 0.0383 0.5644 0.4458 0.047 Uiso d G 1
H H5B -0.022 0.602 0.456 0.047 Uiso d G 1
C C1 0.10470(17) 0.5238(2) 0.26323(19) 0.0237(8) Uani d . 1
H H1A 0.0763 0.5546 0.2124 0.028 Uiso calc R 1
H H1B 0.0839 0.5335 0.3095 0.028 Uiso calc R 1
C C2 0.10835(17) 0.4210(2) 0.24685(18) 0.0214(8) Uani d . 1
C C3 0.05847(17) 0.3756(3) 0.18642(19) 0.0263(9) Uani d . 1
H H3 0.0228 0.4097 0.1507 0.032 Uiso calc R 1
C C4 0.06198(18) 0.2804(3) 0.1795(2) 0.0301(9) Uani d . 1
H H4 0.0283 0.2479 0.1391 0.036 Uiso calc R 1
C C5 0.11492(18) 0.2322(2) 0.23175(19) 0.0262(8) Uani d . 1
H H5 0.1178 0.1664 0.2282 0.031 Uiso calc R 1
C C6 0.16312(17) 0.2817(2) 0.28877(18) 0.0223(8) Uani d . 1
H H6 0.1999 0.2488 0.3238 0.027 Uiso calc R 1
C C7 0.19664(17) 0.5780(3) 0.21132(19) 0.0282(9) Uani d . 1
H H7A 0.2034 0.6453 0.2037 0.034 Uiso calc R 1
H H7B 0.1615 0.5565 0.1615 0.034 Uiso calc R 1
C C8 0.26071(16) 0.5276(2) 0.21309(17) 0.0205(8) Uani d . 1
C C9 0.28912(17) 0.5404(2) 0.14735(18) 0.0232(8) Uani d . 1
H H9 0.2686 0.5807 0.1021 0.028 Uiso calc R 1
C C10 0.34729(18) 0.4943(2) 0.14809(19) 0.0261(9) Uani d . 1
H H10 0.3672 0.5025 0.1035 0.031 Uiso calc R 1
C C11 0.37652(18) 0.4357(2) 0.21491(18) 0.0260(8) Uani d . 1
H H11 0.4166 0.4032 0.2171 0.031 Uiso calc R 1
C C12 0.34536(17) 0.4261(2) 0.27805(18) 0.0233(8) Uani d . 1
H H12 0.3648 0.386 0.3237 0.028 Uiso calc R 1
C C13 0.17209(17) 0.6551(2) 0.3317(2) 0.0255(8) Uani d . 1
H H13A 0.1438 0.6485 0.3705 0.031 Uiso calc R 1
H H13B 0.153 0.7052 0.2912 0.031 Uiso calc R 1
C C14 0.24231(17) 0.6816(2) 0.38129(18) 0.0219(8) Uani d . 1
C C15 0.26103(18) 0.7742(2) 0.39504(18) 0.0258(8) Uani d . 1
H H15 0.2309 0.8224 0.3701 0.031 Uiso calc R 1
C C16 0.32436(17) 0.7959(3) 0.44569(18) 0.0264(9) Uani d . 1
H H16 0.3375 0.8589 0.4571 0.032 Uiso calc R 1
C C17 0.36763(17) 0.7246(2) 0.47901(18) 0.0234(8) Uani d . 1
H H17 0.4114 0.7376 0.5131 0.028 Uiso calc R 1
C C18 0.34617(17) 0.6336(2) 0.46192(18) 0.0212(8) Uani d . 1
H H18 0.3765 0.5846 0.4841 0.025 Uiso calc R 1
C C19 0.13411(18) 0.4252(2) 0.47671(18) 0.0219(8) Uani d . 1
C C20 0.15716(17) 0.3271(2) 0.49505(17) 0.0197(8) Uani d . 1
H H20 0.2027 0.3136 0.5005 0.024 Uiso calc R 1
C C21 0.11798(16) 0.2581(2) 0.50417(17) 0.0193(8) Uani d . 1
H H21 0.0727 0.2716 0.5003 0.023 Uiso calc R 1
C C22 0.14137(18) 0.1596(2) 0.52026(18) 0.0210(8) Uani d . 1
O O7 1.00143(12) 0.09395(19) 0.91564(11) 0.0393(7) Uani d G 1
H H7C 0.9878 0.1446 0.8873 0.059 Uiso d G 1
H H7D 0.9753 0.0811 0.9469 0.059 Uiso d G 1
O O8 1.00220(13) 0.07141(19) 0.16589(11) 0.0472(8) Uani d G 1
H H8A 1.0068 0.0139 0.1521 0.071 Uiso d G 1
H H8B 0.9699 0.0975 0.1274 0.071 Uiso d G 1
O O2 0.20357(11) 0.14732(16) 0.55472(13) 0.0248(6) Uani d . 1
O O6 0.97265(13) 0.25176(18) 0.81730(14) 0.0395(7) Uiso d G 1
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Mn1 O1 7_556 . 99.28(8)
O2 Mn1 N1 7_556 . 95.99(9)
O1 Mn1 N1 . . 163.69(9)
O2 Mn1 N3 7_556 . 118.79(10)
O1 Mn1 N3 . . 92.13(9)
N1 Mn1 N3 . . 85.46(9)
O2 Mn1 N4 7_556 . 93.98(10)
O1 Mn1 N4 . . 87.12(9)
N1 Mn1 N4 . . 86.16(9)
N3 Mn1 N4 . . 146.82(9)
O2 Mn1 N2 7_556 . 164.98(9)
O1 Mn1 N2 . . 87.74(9)
N1 Mn1 N2 . . 76.09(9)
N3 Mn1 N2 . . 73.84(9)
N4 Mn1 N2 . . 72.99(10)
C7 N2 C1 . . 111.2(2)
C7 N2 C13 . . 112.4(3)
C1 N2 C13 . . 110.7(3)
C7 N2 Mn1 . . 110.8(2)
C1 N2 Mn1 . . 106.46(18)
C13 N2 Mn1 . . 104.84(18)
C2 N4 C6 . . 118.0(3)
C2 N4 Mn1 . . 116.0(2)
C6 N4 Mn1 . . 125.8(2)
C12 N1 C8 . . 118.8(3)
C12 N1 Mn1 . . 123.99(19)
C8 N1 Mn1 . . 117.1(2)
C14 N3 C18 . . 117.7(3)
C14 N3 Mn1 . . 115.5(2)
C18 N3 Mn1 . . 126.8(2)
C19 O1 Mn1 . . 129.4(2)
H5A O5 H5B . . 109.6
N2 C1 C2 . . 111.1(3)
N2 C1 H1A . . 109.4
C2 C1 H1A . . 109.4
N2 C1 H1B . . 109.4
C2 C1 H1B . . 109.4
H1A C1 H1B . . 108.0
N4 C2 C3 . . 122.3(3)
N4 C2 C1 . . 116.1(3)
C3 C2 C1 . . 121.5(3)
C4 C3 C2 . . 118.6(3)
C4 C3 H3 . . 120.7
C2 C3 H3 . . 120.7
C3 C4 C5 . . 119.8(3)
C3 C4 H4 . . 120.1
C5 C4 H4 . . 120.1
C6 C5 C4 . . 118.5(3)
C6 C5 H5 . . 120.8
C4 C5 H5 . . 120.8
N4 C6 C5 . . 122.9(3)
N4 C6 H6 . . 118.6
C5 C6 H6 . . 118.6
N2 C7 C8 . . 116.2(3)
N2 C7 H7A . . 108.2
C8 C7 H7A . . 108.2
N2 C7 H7B . . 108.2
C8 C7 H7B . . 108.2
H7A C7 H7B . . 107.4
N1 C8 C9 . . 121.3(3)
N1 C8 C7 . . 119.5(3)
C9 C8 C7 . . 119.2(3)
C10 C9 C8 . . 119.6(3)
C10 C9 H9 . . 120.2
C8 C9 H9 . . 120.2
C9 C10 C11 . . 119.3(3)
C9 C10 H10 . . 120.4
C11 C10 H10 . . 120.4
C12 C11 C10 . . 117.9(3)
C12 C11 H11 . . 121.1
C10 C11 H11 . . 121.1
N1 C12 C11 . . 123.1(3)
N1 C12 H12 . . 118.4
C11 C12 H12 . . 118.4
N2 C13 C14 . . 111.1(3)
N2 C13 H13A . . 109.4
C14 C13 H13A . . 109.4
N2 C13 H13B . . 109.4
C14 C13 H13B . . 109.4
H13A C13 H13B . . 108.0
N3 C14 C15 . . 122.1(3)
N3 C14 C13 . . 116.7(3)
C15 C14 C13 . . 121.0(3)
C14 C15 C16 . . 119.4(3)
C14 C15 H15 . . 120.3
C16 C15 H15 . . 120.3
C17 C16 C15 . . 119.0(3)
C17 C16 H16 . . 120.5
C15 C16 H16 . . 120.5
C16 C17 C18 . . 118.7(3)
C16 C17 H17 . . 120.6
C18 C17 H17 . . 120.6
N3 C18 C17 . . 123.0(3)
N3 C18 H18 . . 118.5
C17 C18 H18 . . 118.5
O4 C19 O1 . . 122.9(3)
O4 C19 C20 . . 119.6(3)
O1 C19 C20 . . 117.6(3)
C21 C20 C19 . . 123.9(3)
C21 C20 H20 . . 118.1
C19 C20 H20 . . 118.1
C20 C21 C22 . . 123.3(3)
C20 C21 H21 . . 118.4
C22 C21 H21 . . 118.4
O3 C22 O2 . . 124.9(3)
O3 C22 C21 . . 118.2(3)
O2 C22 C21 . . 116.9(3)
H7C O7 H7D . . 109.5
H8A O8 H8B . . 109.6
C22 O2 Mn1 . 7_556 132.7(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O2 7_556 2.088(2)
Mn1 O1 . 2.133(2)
Mn1 N1 . 2.244(3)
Mn1 N3 . 2.265(3)
Mn1 N4 . 2.303(3)
Mn1 N2 . 2.354(3)
N2 C7 . 1.474(4)
N2 C1 . 1.480(4)
N2 C13 . 1.483(4)
N4 C2 . 1.348(4)
N4 C6 . 1.352(4)
N1 C12 . 1.344(4)
N1 C8 . 1.345(4)
N3 C14 . 1.349(4)
N3 C18 . 1.358(4)
O1 C19 . 1.277(4)
O4 C19 . 1.247(4)
O3 C22 . 1.245(4)
O5 H5A . 0.8701
O5 H5B . 0.8701
C1 C2 . 1.508(5)
C1 H1A . 0.99
C1 H1B . 0.99
C2 C3 . 1.391(5)
C3 C4 . 1.376(5)
C3 H3 . 0.95
C4 C5 . 1.387(5)
C4 H4 . 0.95
C5 C6 . 1.374(5)
C5 H5 . 0.95
C6 H6 . 0.95
C7 C8 . 1.515(5)
C7 H7A . 0.99
C7 H7B . 0.99
C8 C9 . 1.389(4)
C9 C10 . 1.380(5)
C9 H9 . 0.95
C10 C11 . 1.391(5)
C10 H10 . 0.95
C11 C12 . 1.383(4)
C11 H11 . 0.95
C12 H12 . 0.95
C13 C14 . 1.518(5)
C13 H13A . 0.99
C13 H13B . 0.99
C14 C15 . 1.387(5)
C15 C16 . 1.392(5)
C15 H15 . 0.95
C16 C17 . 1.376(5)
C16 H16 . 0.95
C17 C18 . 1.386(5)
C17 H17 . 0.95
C18 H18 . 0.95
C19 C20 . 1.492(4)
C20 C21 . 1.321(4)
C20 H20 . 0.95
C21 C22 . 1.496(4)
C21 H21 . 0.95
C22 O2 . 1.279(4)
O7 H7C . 0.87
O7 H7D . 0.8701
O8 H8A . 0.8701
O8 H8B . 0.8753
O2 Mn1 7_556 2.088(2)
