#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:27:03 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180435 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/04/7210400.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_7210400
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 H36 N8 Mn2 O8, 6 (H2 O)'
_chemical_formula_sum            'C44 H48 Mn2 N8 O14'
_chemical_formula_weight         1022.78
_chemical_name_common            '[Mn2(tpa)2(adc)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                 101.4770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8422(6)
_cell_length_b                   13.8805(4)
_cell_length_c                   17.2350(5)
_cell_measurement_reflns_used    432
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.4981
_cell_measurement_theta_min      3.1707
_cell_volume                     4651.9(2)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0122
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29607
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         2.05
_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'block shaped'
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0267
_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)+(0.0425P)²+9.1631P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                3725
_reflns_number_total             4060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40882e.txt
_cod_data_source_block           1
_cod_database_code               7210400
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 0.276152(12) 0.534644(17) 0.145436(14) 0.01781(9) Uani d . 1
N N4 0.36311(7) 0.61384(10) 0.23077(8) 0.0222(3) Uani d . 1
N N2 0.33644(7) 0.41813(10) 0.22938(8) 0.0183(3) Uani d . 1
N N1 0.21228(7) 0.51474(9) 0.23740(8) 0.0193(3) Uani d . 1
N N3 0.22842(7) 0.38821(10) 0.10056(8) 0.0201(3) Uani d . 1
O O2 0.23791(7) 0.67706(9) 0.11614(8) 0.0334(3) Uani d . 1
O O1 0.34553(6) 0.50899(8) 0.06839(7) 0.0249(3) Uani d . 1
O O3 0.15866(9) 0.59994(10) 0.02993(8) 0.0452(4) Uani d . 1
O O4 0.41295(6) 0.51803(8) -0.01936(7) 0.0268(3) Uani d . 1
O O5 0.48669(7) 0.36873(9) 0.07021(8) 0.0301(3) Uani d . 1
H H5A 0.5232(13) 0.3921(17) 0.0563(13) 0.045 Uiso d . 1
H H5B 0.4543(12) 0.4033(18) 0.0472(14) 0.045 Uiso d . 1
O O6 0.48076(11) 0.91667(17) 0.95739(16) 0.0956(8) Uani d . 1
O O7 0.01312(8) 0.71028(11) 0.17062(9) 0.0395(3) Uani d . 1
H H7B 0.0107(13) 0.667(2) 0.1272(15) 0.059 Uiso d . 1
H H7C 0.0013(13) 0.761(2) 0.1410(16) 0.059 Uiso d . 1
C C1 0.41098(8) 0.55797(12) 0.27507(9) 0.0208(3) Uani d . 1
C C2 0.40823(8) 0.45248(12) 0.25328(10) 0.0204(3) Uani d . 1
H H2A 0.4326 0.4423 0.2091 0.025 Uiso calc R 1
H H2B 0.4321 0.4144 0.2992 0.025 Uiso calc R 1
C C3 0.30512(8) 0.40578(12) 0.29990(9) 0.0219(4) Uani d . 1
H H3A 0.337 0.433 0.3463 0.026 Uiso calc R 1
H H3B 0.301 0.3359 0.3096 0.026 Uiso calc R 1
C C4 0.23519(8) 0.45143(11) 0.29543(9) 0.0190(3) Uani d . 1
C C5 0.15058(9) 0.55636(12) 0.23499(10) 0.0231(4) Uani d . 1
H H5 0.134 0.6005 0.1934 0.028 Uiso calc R 1
C C6 0.11048(9) 0.53803(13) 0.28984(11) 0.0271(4) Uani d . 1
H H6 0.0673 0.569 0.2864 0.033 Uiso calc R 1
C C7 0.13453(9) 0.47326(13) 0.35046(10) 0.0277(4) Uani d . 1
H H7 0.1082 0.4592 0.3894 0.033 Uiso calc R 1
C C8 0.19756(9) 0.42956(12) 0.35303(10) 0.0238(4) Uani d . 1
H H8 0.215 0.3849 0.3939 0.029 Uiso calc R 1
C C9 0.33426(8) 0.32854(11) 0.18235(10) 0.0215(3) Uani d . 1
H H9A 0.3465 0.2734 0.2188 0.026 Uiso calc R 1
H H9B 0.3691 0.3327 0.1485 0.026 Uiso calc R 1
C C10 0.26470(8) 0.31033(12) 0.13067(9) 0.0202(3) Uani d . 1
C C11 0.16822(9) 0.37388(12) 0.05020(9) 0.0228(4) Uani d . 1
H H11 0.1419 0.4286 0.0293 0.027 Uiso calc R 1
C C12 0.14278(9) 0.28349(13) 0.02740(10) 0.0268(4) Uani d . 1
H H12 0.1002 0.2763 -0.0087 0.032 Uiso calc R 1
C C13 0.18043(9) 0.20350(13) 0.05802(10) 0.0282(4) Uani d . 1
H H13 0.1644 0.1404 0.043 0.034 Uiso calc R 1
C C14 0.24192(9) 0.21717(12) 0.11090(10) 0.0243(4) Uani d . 1
H H14 0.2683 0.1634 0.1335 0.029 Uiso calc R 1
C C15 0.46249(9) 0.59538(13) 0.33398(10) 0.0251(4) Uani d . 1
H H15 0.4945 0.5538 0.366 0.03 Uiso calc R 1
C C16 0.46643(10) 0.69420(14) 0.34538(11) 0.0297(4) Uani d . 1
H H16 0.5015 0.7215 0.3849 0.036 Uiso calc R 1
C C17 0.41845(10) 0.75227(13) 0.29826(11) 0.0305(4) Uani d . 1
H H17 0.4206 0.8203 0.3039 0.037 Uiso calc R 1
C C18 0.36738(9) 0.70961(12) 0.24281(11) 0.0271(4) Uani d . 1
H H18 0.3337 0.7497 0.2117 0.032 Uiso calc R 1
C C19 0.18869(10) 0.67325(12) 0.05851(10) 0.0254(4) Uani d . 1
C C20 0.16464(9) 0.76696(12) 0.02338(9) 0.0225(4) Uani d . 1
C C21 0.35234(8) 0.65404(12) 0.00075(9) 0.0210(3) Uani d . 1
C C22 0.37155(8) 0.55294(12) 0.01894(9) 0.0191(3) Uani 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
O1 Mn1 O2 . 104.52(5)
O1 Mn1 N1 . 162.20(5)
O2 Mn1 N1 . 93.27(5)
O1 Mn1 N3 . 85.22(5)
O2 Mn1 N3 . 129.12(5)
N1 Mn1 N3 . 82.88(5)
O1 Mn1 N4 . 89.02(5)
O2 Mn1 N4 . 84.01(5)
N1 Mn1 N4 . 93.69(5)
N3 Mn1 N4 . 146.75(5)
O1 Mn1 N2 . 87.44(5)
O2 Mn1 N2 . 154.07(5)
N1 Mn1 N2 . 76.57(5)
N3 Mn1 N2 . 73.94(5)
N4 Mn1 N2 . 73.11(5)
C1 N4 C18 . 117.90(15)
C1 N4 Mn1 . 116.23(11)
C18 N4 Mn1 . 125.75(12)
C9 N2 C2 . 110.15(12)
C9 N2 C3 . 112.38(13)
C2 N2 C3 . 110.27(12)
C9 N2 Mn1 . 106.68(9)
C2 N2 Mn1 . 107.18(9)
C3 N2 Mn1 . 109.99(9)
C4 N1 C5 . 118.38(14)
C4 N1 Mn1 . 117.00(11)
C5 N1 Mn1 . 124.43(11)
C11 N3 C10 . 117.96(14)
C11 N3 Mn1 . 126.79(11)
C10 N3 Mn1 . 115.21(10)
C19 O2 Mn1 . 109.45(12)
C22 O1 Mn1 . 139.18(11)
H5A O5 H5B . 105.(2)
H7B O7 H7C . 95.(2)
N4 C1 C15 . 122.31(16)
N4 C1 C2 . 115.64(14)
C15 C1 C2 . 121.93(15)
N2 C2 C1 . 111.50(13)
N2 C2 H2A . 109.3
C1 C2 H2A . 109.3
N2 C2 H2B . 109.3
C1 C2 H2B . 109.3
H2A C2 H2B . 108.0
N2 C3 C4 . 116.10(13)
N2 C3 H3A . 108.3
C4 C3 H3A . 108.3
N2 C3 H3B . 108.3
C4 C3 H3B . 108.3
H3A C3 H3B . 107.4
N1 C4 C8 . 121.69(15)
N1 C4 C3 . 118.93(14)
C8 C4 C3 . 119.33(14)
N1 C5 C6 . 123.11(16)
N1 C5 H5 . 118.4
C6 C5 H5 . 118.4
C5 C6 C7 . 118.53(16)
C5 C6 H6 . 120.7
C7 C6 H6 . 120.7
C8 C7 C6 . 118.78(16)
C8 C7 H7 . 120.6
C6 C7 H7 . 120.6
C7 C8 C4 . 119.50(16)
C7 C8 H8 . 120.2
C4 C8 H8 . 120.2
N2 C9 C10 . 112.83(13)
N2 C9 H9A . 109.0
C10 C9 H9A . 109.0
N2 C9 H9B . 109.0
C10 C9 H9B . 109.0
H9A C9 H9B . 107.8
N3 C10 C14 . 122.04(15)
N3 C10 C9 . 116.75(14)
C14 C10 C9 . 121.05(15)
N3 C11 C12 . 123.10(16)
N3 C11 H11 . 118.5
C12 C11 H11 . 118.5
C11 C12 C13 . 118.82(16)
C11 C12 H12 . 120.6
C13 C12 H12 . 120.6
C14 C13 C12 . 118.69(16)
C14 C13 H13 . 120.7
C12 C13 H13 . 120.7
C13 C14 C10 . 119.37(16)
C13 C14 H14 . 120.3
C10 C14 H14 . 120.3
C16 C15 C1 . 119.06(17)
C16 C15 H15 . 120.5
C1 C15 H15 . 120.5
C17 C16 C15 . 118.79(17)
C17 C16 H16 . 120.6
C15 C16 H16 . 120.6
C18 C17 C16 . 118.81(17)
C18 C17 H17 . 120.6
C16 C17 H17 . 120.6
N4 C18 C17 . 123.06(17)
N4 C18 H18 . 118.5
C17 C18 H18 . 118.5
O3 C19 O2 . 126.39(17)
O3 C19 C20 . 118.27(16)
O2 C19 C20 . 115.34(16)
C21 C20 C19 7_565 175.60(18)
C20 C21 C22 7_565 172.15(17)
O1 C22 O4 . 125.40(15)
O1 C22 C21 . 119.31(15)
O4 C22 C21 . 115.27(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O1 . 2.1242(12)
Mn1 O2 . 2.1415(13)
Mn1 N1 . 2.2349(14)
Mn1 N3 . 2.3097(13)
Mn1 N4 . 2.3106(14)
Mn1 N2 . 2.3346(13)
N4 C1 . 1.341(2)
N4 C18 . 1.346(2)
N2 C9 . 1.480(2)
N2 C2 . 1.481(2)
N2 C3 . 1.481(2)
N1 C4 . 1.341(2)
N1 C5 . 1.347(2)
N3 C11 . 1.344(2)
N3 C10 . 1.344(2)
O2 C19 . 1.248(2)
O1 C22 . 1.241(2)
O3 C19 . 1.232(2)
O4 C22 . 1.249(2)
O5 H5A . 0.87(2)
O5 H5B . 0.84(3)
O7 H7B . 0.96(3)
O7 H7C . 0.88(3)
C1 C15 . 1.390(2)
C1 C2 . 1.510(2)
C2 H2A . 0.99
C2 H2B . 0.99
C3 C4 . 1.513(2)
C3 H3A . 0.99
C3 H3B . 0.99
C4 C8 . 1.389(2)
C5 C6 . 1.375(3)
C5 H5 . 0.95
C6 C7 . 1.389(3)
C6 H6 . 0.95
C7 C8 . 1.383(3)
C7 H7 . 0.95
C8 H8 . 0.95
C9 C10 . 1.508(2)
C9 H9A . 0.99
C9 H9B . 0.99
C10 C14 . 1.390(2)
C11 C12 . 1.380(2)
C11 H11 . 0.95
C12 C13 . 1.383(3)
C12 H12 . 0.95
C13 C14 . 1.383(3)
C13 H13 . 0.95
C14 H14 . 0.95
C15 C16 . 1.386(3)
C15 H15 . 0.95
C16 C17 . 1.381(3)
C16 H16 . 0.95
C17 C18 . 1.380(3)
C17 H17 . 0.95
C18 H18 . 0.95
C19 C20 . 1.474(2)
C20 C21 7_565 1.197(2)
C21 C20 7_565 1.197(2)
C21 C22 . 1.471(2)
