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#$Date: 2025-08-21 03:19:08 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301842 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/68/4506836.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_4506836
loop_
_publ_author_name
'Khullar, Sadhika'
'Mandal, Sanjay K.'
_publ_section_title
;
 Supramolecular Assemblies of Dimanganese Subunits and Water Clusters
 Organized by Strong Hydrogen Bonding Interactions: Single Crystal to
 Single Crystal Transformation by Thermal De-/Rehydration Processes
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5329
_journal_paper_doi               10.1021/cg300937f
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C40 H46 Mn2 N6 O10, 6(H2 O)'
_chemical_formula_sum            'C40 H58 Mn2 N6 O16'
_chemical_formula_weight         988.80
_chemical_name_common            '[Mn2(adc)2(bpta)2(H2O)2].6H2O'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.477(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1371(5)
_cell_length_b                   17.3888(9)
_cell_length_c                   13.9458(7)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    120.(2)
_cell_measurement_theta_max      25.0791
_cell_measurement_theta_min      2.4318
_cell_volume                     2317.6(2)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker)'
_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      120.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25564
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.372
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4124
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0767P)²+0.8092P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                3552
_reflns_number_total             4124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300937f_si_002.cif
_cod_data_source_block           1.6H2O
_cod_database_code               4506836
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.18195(3) 0.141771(19) 0.01349(3) 0.01656(15) Uani d . 1
N N1 0.1811(2) 0.27895(11) 0.05073(14) 0.0176(4) Uani d . 1
N N2 -0.04348(19) 0.17312(12) -0.01249(14) 0.0185(4) Uani d . 1
N N3 0.2299(2) 0.20336(11) -0.11267(14) 0.0174(4) Uani d . 1
O O1 0.1855(2) 0.09453(11) 0.15723(13) 0.0266(4) Uani d . 1
H H1B 0.2523 0.0634 0.1784 0.04 Uiso calc R 1
H H1A 0.127(4) 0.075(2) 0.172(3) 0.048(11) Uiso d . 1
O O5 0.39868(17) 0.10878(10) 0.05983(12) 0.0217(4) Uani d . 1
O O4 0.42965(19) 0.02356(11) 0.18598(15) 0.0366(5) Uani d . 1
O O2 0.10478(17) 0.04316(10) -0.08010(13) 0.0246(4) Uani d . 1
O O3 0.04058(18) -0.04734(11) -0.20001(14) 0.0318(5) Uani d . 1
O O6 0.1075(11) 0.0798(5) 0.3928(8) 0.128(3) Uiso d PD 0.5
H H6A 0.023(5) 0.066(8) 0.385(12) 0.192 Uiso d PD 0.5
H H6B 0.163(11) 0.044(6) 0.425(10) 0.192 Uiso d PD 0.5
O O7 0.6003(4) 0.5016(2) 0.0975(3) 0.1055(13) Uani d D 1
H H7C 0.668(5) 0.478(4) 0.086(5) 0.158 Uiso d D 1
H H7D 0.532(5) 0.505(5) 0.042(3) 0.158 Uiso d D 1
O O8 0.6183(3) 0.96315(15) 0.36360(18) 0.0655(8) Uani d D 1
H H8A 0.577(4) 0.975(3) 0.3010(11) 0.098 Uiso d D 1
H H8B 0.559(4) 0.978(3) 0.391(3) 0.098 Uiso d D 1
O O9 0.4215(6) 0.0395(4) 0.4573(4) 0.0673(16) Uani d PD 0.5
H H9A 0.337(4) 0.053(6) 0.437(6) 0.101 Uiso d PD 0.5
H H9B 0.448(8) 0.027(6) 0.519(2) 0.101 Uiso d PD 0.5
C C1 0.1486(3) 0.31754(14) -0.04982(17) 0.0205(5) Uani d . 1
H H1D 0.1804 0.3716 -0.0386 0.025 Uiso calc R 1
H H1C 0.0458 0.318 -0.0838 0.025 Uiso calc R 1
C C2 0.2150(2) 0.28003(13) -0.11935(17) 0.0188(5) Uani d . 1
C C3 0.2547(3) 0.32279(14) -0.18937(18) 0.0251(6) Uani d . 1
H H3 0.2424 0.377 -0.1931 0.03 Uiso calc R 1
C C4 0.3123(3) 0.28572(15) -0.25341(19) 0.0277(6) Uani d . 1
H H4 0.3394 0.314 -0.3021 0.033 Uiso calc R 1
C C5 0.3301(3) 0.20694(15) -0.24581(18) 0.0236(5) Uani d . 1
H H5 0.3704 0.1801 -0.2885 0.028 Uiso calc R 1
C C6 0.2879(2) 0.16820(14) -0.17456(18) 0.0203(5) Uani d . 1
H H6 0.3006 0.114 -0.1691 0.024 Uiso calc R 1
C C7 0.0579(2) 0.28810(14) 0.08423(18) 0.0216(5) Uani d . 1
H H7B 0.0331 0.3433 0.082 0.026 Uiso calc R 1
H H7A 0.0827 0.2706 0.1556 0.026 Uiso calc R 1
C C8 -0.0679(2) 0.24328(14) 0.01915(17) 0.0193(5) Uani d . 1
C C9 -0.2021(3) 0.27167(16) -0.00187(18) 0.0262(6) Uani d . 1
H H9 -0.2165 0.3222 0.0185 0.031 Uiso calc R 1
C C10 -0.3157(3) 0.22549(16) -0.05310(19) 0.0285(6) Uani d . 1
H H10 -0.4087 0.2437 -0.0674 0.034 Uiso calc R 1
C C11 -0.2911(3) 0.15256(15) -0.08280(19) 0.0257(6) Uani d . 1
H H11 -0.3668 0.1193 -0.1165 0.031 Uiso calc R 1
C C12 -0.1544(3) 0.12895(15) -0.06252(18) 0.0221(5) Uani d . 1
H H12 -0.1377 0.0794 -0.0848 0.026 Uiso calc R 1
C C13 0.3134(3) 0.31061(14) 0.12944(18) 0.0215(5) Uani d . 1
C C14 0.4329(3) 0.30976(16) 0.0855(2) 0.0284(6) Uani d . 1
H H14C 0.52 0.3253 0.1382 0.043 Uiso calc R 1
H H14B 0.4117 0.3457 0.0282 0.043 Uiso calc R 1
H H14A 0.4435 0.2578 0.062 0.043 Uiso calc R 1
C C15 0.2937(3) 0.39312(15) 0.1619(2) 0.0314(6) Uani d . 1
H H15A 0.2238 0.3933 0.1964 0.047 Uiso calc R 1
H H15B 0.2617 0.4262 0.1016 0.047 Uiso calc R 1
H H15C 0.3829 0.4125 0.2083 0.047 Uiso calc R 1
C C16 0.3558(3) 0.25833(15) 0.22282(18) 0.0253(6) Uani d . 1
H H16A 0.3739 0.2064 0.203 0.038 Uiso calc R 1
H H16B 0.2799 0.2565 0.2517 0.038 Uiso calc R 1
H H16C 0.4406 0.2786 0.2737 0.038 Uiso calc R 1
C C17 0.4672(2) 0.05899(14) 0.12149(18) 0.0209(5) Uani d . 1
C C18 0.6073(2) 0.04136(13) 0.11856(18) 0.0187(5) Uani d . 1
C C19 0.2764(2) -0.02604(13) -0.12200(18) 0.0196(5) Uani d . 1
C C20 0.1295(2) -0.00838(13) -0.13425(18) 0.0198(5) 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
O2 Mn1 O5 . 95.66(6)
O2 Mn1 O1 . 98.70(7)
O5 Mn1 O1 . 85.43(7)
O2 Mn1 N3 . 92.00(7)
O5 Mn1 N3 . 84.06(7)
O1 Mn1 N3 . 165.68(7)
O2 Mn1 N2 . 87.19(7)
O5 Mn1 N2 . 172.00(7)
O1 Mn1 N2 . 86.75(7)
N3 Mn1 N2 . 103.34(7)
O2 Mn1 N1 . 152.42(7)
O5 Mn1 N1 . 105.81(6)
O1 Mn1 N1 . 100.06(7)
N3 Mn1 N1 . 73.62(7)
N2 Mn1 N1 . 73.92(7)
C7 N1 C1 . 107.68(18)
C7 N1 C13 . 111.47(18)
C1 N1 C13 . 112.38(18)
C7 N1 Mn1 . 103.61(14)
C1 N1 Mn1 . 104.79(13)
C13 N1 Mn1 . 116.17(14)
C8 N2 C12 . 118.2(2)
C8 N2 Mn1 . 116.90(15)
C12 N2 Mn1 . 124.76(17)
C2 N3 C6 . 118.1(2)
C2 N3 Mn1 . 118.65(15)
C6 N3 Mn1 . 122.81(15)
Mn1 O1 H1B . 109.5
Mn1 O1 H1A . 130.(3)
H1B O1 H1A . 102.6
C17 O5 Mn1 . 131.84(16)
C20 O2 Mn1 . 146.84(16)
H6A O6 H6B . 109.(3)
H7C O7 H7D . 109.(3)
H8A O8 H8B . 102.(2)
H9A O9 H9B . 111.(3)
N1 C1 C2 . 113.97(19)
N1 C1 H1D . 108.8
C2 C1 H1D . 108.8
N1 C1 H1C . 108.8
C2 C1 H1C . 108.8
H1D C1 H1C . 107.7
N3 C2 C3 . 121.9(2)
N3 C2 C1 . 116.8(2)
C3 C2 C1 . 121.3(2)
C4 C3 C2 . 119.3(2)
C4 C3 H3 . 120.3
C2 C3 H3 . 120.3
C3 C4 C5 . 119.1(2)
C3 C4 H4 . 120.4
C5 C4 H4 . 120.4
C4 C5 C6 . 118.4(2)
C4 C5 H5 . 120.8
C6 C5 H5 . 120.8
N3 C6 C5 . 123.2(2)
N3 C6 H6 . 118.4
C5 C6 H6 . 118.4
N1 C7 C8 . 112.74(19)
N1 C7 H7B . 109.0
C8 C7 H7B . 109.0
N1 C7 H7A . 109.0
C8 C7 H7A . 109.0
H7B C7 H7A . 107.8
N2 C8 C9 . 121.9(2)
N2 C8 C7 . 116.9(2)
C9 C8 C7 . 121.1(2)
C8 C9 C10 . 119.4(2)
C8 C9 H9 . 120.3
C10 C9 H9 . 120.3
C11 C10 C9 . 118.9(2)
C11 C10 H10 . 120.6
C9 C10 H10 . 120.6
C12 C11 C10 . 118.7(2)
C12 C11 H11 . 120.6
C10 C11 H11 . 120.6
N2 C12 C11 . 122.9(2)
N2 C12 H12 . 118.5
C11 C12 H12 . 118.5
N1 C13 C16 . 109.20(19)
N1 C13 C14 . 109.41(19)
C16 C13 C14 . 107.5(2)
N1 C13 C15 . 112.3(2)
C16 C13 C15 . 109.4(2)
C14 C13 C15 . 109.0(2)
C13 C14 H14C . 109.5
C13 C14 H14B . 109.5
H14C C14 H14B . 109.5
C13 C14 H14A . 109.5
H14C C14 H14A . 109.5
H14B C14 H14A . 109.5
C13 C15 H15A . 109.5
C13 C15 H15B . 109.5
H15A C15 H15B . 109.5
C13 C15 H15C . 109.5
H15A C15 H15C . 109.5
H15B C15 H15C . 109.5
C13 C16 H16A . 109.5
C13 C16 H16B . 109.5
H16A C16 H16B . 109.5
C13 C16 H16C . 109.5
H16A C16 H16C . 109.5
H16B C16 H16C . 109.5
O4 C17 O5 . 127.0(2)
O4 C17 C18 . 116.6(2)
O5 C17 C18 . 116.5(2)
C19 C18 C17 3_655 176.2(2)
C18 C19 C20 3_655 175.8(2)
O3 C20 O2 . 126.2(2)
O3 C20 C19 . 115.2(2)
O2 C20 C19 . 118.5(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O2 . 2.1389(17)
Mn1 O5 . 2.1510(16)
Mn1 O1 . 2.1556(19)
Mn1 N3 . 2.2468(19)
Mn1 N2 . 2.2580(19)
Mn1 N1 . 2.4420(19)
N1 C7 . 1.480(3)
N1 C1 . 1.489(3)
N1 C13 . 1.525(3)
N2 C8 . 1.348(3)
N2 C12 . 1.348(3)
N3 C2 . 1.342(3)
N3 C6 . 1.343(3)
O1 H1B . 0.84
O1 H1A . 0.78(4)
O5 C17 . 1.254(3)
O4 C17 . 1.250(3)
O2 C20 . 1.250(3)
O3 C20 . 1.249(3)
O6 H6A . 0.858(10)
O6 H6B . 0.856(10)
O7 H7C . 0.858(10)
O7 H7D . 0.846(10)
O8 H8A . 0.859(10)
O8 H8B . 0.856(10)
O9 H9A . 0.847(10)
O9 H9B . 0.847(10)
C1 C2 . 1.502(3)
C1 H1D . 0.99
C1 H1C . 0.99
C2 C3 . 1.389(3)
C3 C4 . 1.379(4)
C3 H3 . 0.95
C4 C5 . 1.381(4)
C4 H4 . 0.95
C5 C6 . 1.381(3)
C5 H5 . 0.95
C6 H6 . 0.95
C7 C8 . 1.512(3)
C7 H7B . 0.99
C7 H7A . 0.99
C8 C9 . 1.384(3)
C9 C10 . 1.390(4)
C9 H9 . 0.95
C10 C11 . 1.382(4)
C10 H10 . 0.95
C11 C12 . 1.382(4)
C11 H11 . 0.95
C12 H12 . 0.95
C13 C16 . 1.528(3)
C13 C14 . 1.529(4)
C13 C15 . 1.537(4)
C14 H14C . 0.98
C14 H14B . 0.98
C14 H14A . 0.98
C15 H15A . 0.98
C15 H15B . 0.98
C15 H15C . 0.98
C16 H16A . 0.98
C16 H16B . 0.98
C16 H16C . 0.98
C17 C18 . 1.466(3)
C18 C19 3_655 1.194(3)
C19 C18 3_655 1.194(3)
C19 C20 . 1.474(3)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139146233
