#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:27:03 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180435 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/04/7210402.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_7210402
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 H44 Mn2 N8 O8, 6 (H2 O)'
_chemical_formula_sum            'C44 H56 Mn2 N8 O14'
_chemical_formula_weight         1030.85
_chemical_name_common            '[Mn2(tpa)2(succinate)2].6H2O'
_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                 101.871(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7966(15)
_cell_length_b                   13.7795(11)
_cell_length_c                   17.1799(13)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.1322
_cell_measurement_theta_min      2.8485
_cell_volume                     4586.2(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0100
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26788
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'block shaped'
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.955
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0576P)²+26.5215P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                3995
_reflns_number_total             4094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40882e.txt
_cod_data_source_block           3
_cod_database_code               7210402
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 0.237364(19) 0.03823(3) 0.86012(2) 0.01877(14) Uani d . 1
N N1 0.29568(12) 0.01755(17) 0.76159(12) 0.0226(5) Uani d . 1
N N2 0.16939(11) -0.07540(15) 0.77293(13) 0.0196(5) Uani d . 1
N N3 0.14968(11) 0.12300(15) 0.77146(12) 0.0211(5) Uani d . 1
N N4 0.27810(11) -0.11624(16) 0.90074(12) 0.0196(4) Uani d . 1
O O1 0.27716(13) 0.1904(2) 0.88498(14) 0.0519(7) Uani d . 1
O O2 0.16687(9) 0.02232(14) 0.93632(11) 0.0244(4) Uani d . 1
O O3 0.08937(10) 0.04692(14) 1.00975(13) 0.0292(5) Uani d . 1
O O4 0.35051(18) 0.08511(18) 0.94996(14) 0.0617(9) Uani d . 1
O O5 0.01028(9) 0.27493(15) 0.17036(13) 0.0362(5) Uani d G 1
H H5A -0.0024 0.2213 0.1448 0.054 Uiso d G 1
H H5B 0.0035 0.3235 0.1373 0.054 Uiso d G 1
O O7 0.47967(9) 0.61274(14) 0.07167(12) 0.0257(4) Uani d G 1
C C1 0.35752(15) 0.0578(2) 0.76048(16) 0.0285(6) Uani d . 1
H H1 0.3769 0.1008 0.8024 0.034 Uiso calc R 1
C C2 0.39401(16) 0.0400(2) 0.70196(17) 0.0305(7) Uani d . 1
H H2 0.4377 0.0694 0.7038 0.037 Uiso calc R 1
C C3 0.36556(15) -0.0218(2) 0.64019(17) 0.0281(6) Uani d . 1
H H3 0.3892 -0.0354 0.5986 0.034 Uiso calc R 1
C C4 0.30215(15) -0.06311(19) 0.64062(16) 0.0249(6) Uani d . 1
H H4 0.2815 -0.1054 0.5988 0.03 Uiso calc R 1
C C5 0.26838(14) -0.04291(18) 0.70229(15) 0.0207(5) Uani d . 1
C C6 0.19832(13) -0.08741(19) 0.70055(15) 0.0222(5) Uani d . 1
H H6A 0.1653 -0.0591 0.6551 0.027 Uiso calc R 1
H H6B 0.2014 -0.1578 0.69 0.027 Uiso calc R 1
O O6 1.01428(19) 0.4412(2) 0.06785(19) 0.0719(9) Uani d G 1
C C7 0.33724(13) -0.1361(2) 0.95273(15) 0.0225(5) Uani d . 1
H H7 0.3664 -0.0837 0.9742 0.027 Uiso calc R 1
C C8 0.35743(14) -0.2296(2) 0.97626(16) 0.0265(6) Uani d . 1
H H8 0.3993 -0.2407 1.0136 0.032 Uiso calc R 1
C C9 0.31600(15) -0.3064(2) 0.94478(16) 0.0264(6) Uani d . 1
H H9 0.3286 -0.3712 0.9602 0.032 Uiso calc R 1
C C10 0.25569(14) -0.2870(2) 0.89027(16) 0.0239(6) Uani d . 1
H H10 0.2265 -0.3385 0.8669 0.029 Uiso calc R 1
C C11 0.23820(13) -0.19103(19) 0.87000(15) 0.0200(5) Uani d . 1
C C12 0.16914(14) -0.16676(19) 0.81771(17) 0.0260(6) Uani d . 1
H H12A 0.1552 -0.2205 0.7795 0.031 Uiso calc R 1
H H12B 0.1342 -0.1618 0.8513 0.031 Uiso calc R 1
C C13 0.09845(13) -0.03642(18) 0.75149(16) 0.0211(5) Uani d . 1
H H13A 0.0754 -0.0446 0.797 0.025 Uiso calc R 1
H H13B 0.0719 -0.0737 0.706 0.025 Uiso calc R 1
C C14 0.09833(13) 0.06926(19) 0.72951(15) 0.0195(5) Uani d . 1
C C15 0.04547(14) 0.1094(2) 0.67270(16) 0.0245(6) Uani d . 1
H H15 0.0111 0.0691 0.6419 0.029 Uiso calc R 1
C C16 0.04375(16) 0.2089(2) 0.66182(17) 0.0291(6) Uani d . 1
H H16 0.0076 0.2381 0.6242 0.035 Uiso calc R 1
C C17 0.09539(16) 0.2652(2) 0.70643(17) 0.0291(6) Uani d . 1
H H17 0.0948 0.3338 0.701 0.035 Uiso calc R 1
C C18 0.14773(15) 0.21944(19) 0.75904(16) 0.0255(6) Uani d . 1
H H18 0.1842 0.258 0.788 0.031 Uiso calc R 1
C C19 0.13502(13) 0.07720(19) 0.97539(14) 0.0201(5) Uani d . 1
C C20 0.15549(14) 0.1836(2) 0.98138(16) 0.0242(6) Uani d . 1
H H20A 0.1468 0.2111 0.927 0.029 Uiso calc R 1
H H20B 0.2058 0.1876 1.0029 0.029 Uiso calc R 1
C C21 0.38097(14) 0.2526(2) 0.96749(15) 0.0247(6) Uani d . 1
H H21A 0.424 0.2261 1.0003 0.03 Uiso calc R 1
H H21B 0.3933 0.2917 0.9242 0.03 Uiso calc R 1
C C22 0.3333(2) 0.1694(2) 0.93222(18) 0.0415(9) Uani d . 1
H H7A 0.450(2) 0.574(3) 0.050(3) 0.063(13) Uiso d . 1
H H7B 0.513(2) 0.600(3) 0.051(2) 0.047(11) Uiso d . 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 . . 103.25(8)
O2 Mn1 N1 . . 163.31(8)
O1 Mn1 N1 . . 92.69(8)
O2 Mn1 N4 . . 87.23(7)
O1 Mn1 N4 . . 135.06(9)
N1 Mn1 N4 . . 84.86(8)
O2 Mn1 N3 . . 87.68(7)
O1 Mn1 N3 . . 81.04(9)
N1 Mn1 N3 . . 90.01(8)
N4 Mn1 N3 . . 143.64(8)
O2 Mn1 N2 . . 87.81(8)
O1 Mn1 N2 . . 149.58(9)
N1 Mn1 N2 . . 75.83(8)
N4 Mn1 N2 . . 72.79(7)
N3 Mn1 N2 . . 71.06(7)
O2 Mn1 O4 . . 105.27(8)
O1 Mn1 O4 . . 54.15(9)
N1 Mn1 O4 . . 87.97(8)
N4 Mn1 O4 . . 80.91(8)
N3 Mn1 O4 . . 134.95(8)
N2 Mn1 O4 . . 150.05(9)
C5 N1 C1 . . 118.1(2)
C5 N1 Mn1 . . 117.42(18)
C1 N1 Mn1 . . 124.43(18)
C12 N2 C13 . . 109.6(2)
C12 N2 C6 . . 112.7(2)
C13 N2 C6 . . 110.1(2)
C12 N2 Mn1 . . 107.15(15)
C13 N2 Mn1 . . 107.63(15)
C6 N2 Mn1 . . 109.59(15)
C14 N3 C18 . . 117.8(2)
C14 N3 Mn1 . . 116.58(17)
C18 N3 Mn1 . . 125.63(18)
C11 N4 C7 . . 117.8(2)
C11 N4 Mn1 . . 116.42(16)
C7 N4 Mn1 . . 125.77(18)
C22 O1 Mn1 . . 97.8(2)
C19 O2 Mn1 . . 137.17(17)
C22 O4 Mn1 . . 85.7(2)
H5A O5 H5B . . 109.6
H7A O7 H7B . . 103.(4)
N1 C1 C2 . . 123.5(3)
N1 C1 H1 . . 118.2
C2 C1 H1 . . 118.2
C1 C2 C3 . . 118.5(3)
C1 C2 H2 . . 120.7
C3 C2 H2 . . 120.7
C4 C3 C2 . . 118.4(3)
C4 C3 H3 . . 120.8
C2 C3 H3 . . 120.8
C3 C4 C5 . . 120.1(3)
C3 C4 H4 . . 120.0
C5 C4 H4 . . 120.0
N1 C5 C4 . . 121.4(2)
N1 C5 C6 . . 119.5(2)
C4 C5 C6 . . 119.1(2)
N2 C6 C5 . . 116.7(2)
N2 C6 H6A . . 108.1
C5 C6 H6A . . 108.1
N2 C6 H6B . . 108.1
C5 C6 H6B . . 108.1
H6A C6 H6B . . 107.3
N4 C7 C8 . . 122.9(3)
N4 C7 H7 . . 118.6
C8 C7 H7 . . 118.6
C9 C8 C7 . . 119.1(3)
C9 C8 H8 . . 120.4
C7 C8 H8 . . 120.4
C8 C9 C10 . . 118.5(3)
C8 C9 H9 . . 120.7
C10 C9 H9 . . 120.7
C9 C10 C11 . . 119.2(3)
C9 C10 H10 . . 120.4
C11 C10 H10 . . 120.4
N4 C11 C10 . . 122.4(2)
N4 C11 C12 . . 116.9(2)
C10 C11 C12 . . 120.4(2)
N2 C12 C11 . . 113.5(2)
N2 C12 H12A . . 108.9
C11 C12 H12A . . 108.9
N2 C12 H12B . . 108.9
C11 C12 H12B . . 108.9
H12A C12 H12B . . 107.7
N2 C13 C14 . . 111.5(2)
N2 C13 H13A . . 109.3
C14 C13 H13A . . 109.3
N2 C13 H13B . . 109.3
C14 C13 H13B . . 109.3
H13A C13 H13B . . 108.0
N3 C14 C15 . . 122.4(2)
N3 C14 C13 . . 115.9(2)
C15 C14 C13 . . 121.5(2)
C16 C15 C14 . . 118.9(3)
C16 C15 H15 . . 120.6
C14 C15 H15 . . 120.6
C17 C16 C15 . . 119.1(3)
C17 C16 H16 . . 120.5
C15 C16 H16 . . 120.5
C18 C17 C16 . . 118.5(3)
C18 C17 H17 . . 120.7
C16 C17 H17 . . 120.7
N3 C18 C17 . . 123.3(3)
N3 C18 H18 . . 118.4
C17 C18 H18 . . 118.4
O3 C19 O2 . . 122.7(2)
O3 C19 C20 . . 120.0(2)
O2 C19 C20 . . 117.3(2)
C19 C20 C21 . 7_557 116.4(2)
C19 C20 H20A . . 108.2
C21 C20 H20A 7_557 . 108.2
C19 C20 H20B . . 108.2
C21 C20 H20B 7_557 . 108.2
H20A C20 H20B . . 107.4
C20 C21 C22 7_557 . 109.5(2)
C20 C21 H21A 7_557 . 109.8
C22 C21 H21A . . 109.8
C20 C21 H21B 7_557 . 109.8
C22 C21 H21B . . 109.8
H21A C21 H21B . . 108.2
O4 C22 O1 . . 122.4(3)
O4 C22 C21 . . 119.5(3)
O1 C22 C21 . . 118.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O2 . 2.1122(18)
Mn1 O1 . 2.249(3)
Mn1 N1 . 2.255(2)
Mn1 N4 . 2.332(2)
Mn1 N3 . 2.369(2)
Mn1 N2 . 2.383(2)
Mn1 O4 . 2.529(3)
N1 C5 . 1.341(3)
N1 C1 . 1.348(4)
N2 C12 . 1.476(3)
N2 C13 . 1.478(3)
N2 C6 . 1.482(3)
N3 C14 . 1.342(3)
N3 C18 . 1.345(3)
N4 C11 . 1.339(3)
N4 C7 . 1.347(3)
O1 C22 . 1.267(5)
O2 C19 . 1.263(3)
O3 C19 . 1.248(3)
O4 C22 . 1.231(5)
O5 H5A . 0.87
O5 H5B . 0.87
O7 H7A . 0.83(5)
O7 H7B . 0.84(4)
C1 C2 . 1.375(4)
C1 H1 . 0.95
C2 C3 . 1.387(4)
C2 H2 . 0.95
C3 C4 . 1.380(4)
C3 H3 . 0.95
C4 C5 . 1.392(4)
C4 H4 . 0.95
C5 C6 . 1.511(4)
C6 H6A . 0.99
C6 H6B . 0.99
C7 C8 . 1.383(4)
C7 H7 . 0.95
C8 C9 . 1.380(4)
C8 H8 . 0.95
C9 C10 . 1.384(4)
C9 H9 . 0.95
C10 C11 . 1.393(4)
C10 H10 . 0.95
C11 C12 . 1.511(4)
C12 H12A . 0.99
C12 H12B . 0.99
C13 C14 . 1.504(4)
C13 H13A . 0.99
C13 H13B . 0.99
C14 C15 . 1.390(4)
C15 C16 . 1.383(4)
C15 H15 . 0.95
C16 C17 . 1.383(4)
C16 H16 . 0.95
C17 C18 . 1.379(4)
C17 H17 . 0.95
C18 H18 . 0.95
C19 C20 . 1.519(4)
C20 C21 7_557 1.525(4)
C20 H20A . 0.99
C20 H20B . 0.99
C21 C20 7_557 1.525(4)
C21 C22 . 1.529(4)
C21 H21A . 0.99
C21 H21B . 0.99
