#------------------------------------------------------------------------------
#$Date: 2015-08-08 05:32:02 +0300 (Sat, 08 Aug 2015) $
#$Revision: 153209 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/53/7035351.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_7035351
loop_
_publ_author_name
'Phukan, Bedika'
'Patel, Anant B.'
'Mukherjee, Chandan'
_publ_section_title
;
 A water-soluble and water-coordinated Mn(ii) complex: synthesis,
 characterization and phantom MRI image study.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12990
_journal_page_last               12994
_journal_paper_doi               10.1039/c5dt01781e
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C30 H48 Mn4 N4 O26, 8(H2 O)'
_chemical_formula_sum            'C30 H64 Mn4 N4 O34'
_chemical_formula_weight         1244.61
_chemical_name_systematic        unk
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-04 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                71.602(6)
_cell_angle_beta                 64.303(7)
_cell_angle_gamma                77.400(6)
_cell_formula_units_Z            1
_cell_length_a                   10.4029(8)
_cell_length_b                   11.7222(8)
_cell_length_c                   11.8865(7)
_cell_measurement_reflns_used    2865
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5760
_cell_measurement_theta_min      2.9795
_cell_volume                     1233.77(17)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6911
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             644
_exptl_crystal_recrystallization_method water
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0380P)²+0.2337P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                3039
_reflns_number_total             3840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01781e2.cif
_cod_data_source_block           exp_1166
_cod_depositor_comments          'Adding full bibliography for 7035351.cif.'
_cod_original_cell_volume        1233.77(15)
_cod_database_code               7035351
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Mn1 Mn 0.84366(5) 0.30404(5) 0.65131(5) 0.02153(16) Uani 1 1 d .
Mn2 Mn 0.50547(5) 0.74205(5) 0.56894(5) 0.02314(17) Uani 1 1 d .
O8 O 0.5447(2) 0.1424(2) 0.5953(2) 0.0269(6) Uani 1 1 d .
O1 O 0.7158(3) 0.4818(2) 0.6229(2) 0.0313(7) Uani 1 1 d .
O4 O 0.9719(4) 0.4435(3) 0.8740(3) 0.0674(10) Uani 1 1 d .
O2 O 0.5609(3) 0.6187(2) 0.7230(2) 0.0334(7) Uani 1 1 d .
O6 O 1.1676(2) 0.0136(2) 0.5953(2) 0.0364(7) Uani 1 1 d .
O5 O 1.0390(2) 0.1822(2) 0.6452(2) 0.0309(7) Uani 1 1 d .
O13 O 0.7251(2) 0.6932(2) 0.4334(2) 0.0329(7) Uani 1 1 d .
H13A H 0.7578 0.6242 0.4677 0.049 Uiso 1 1 d R
H13B H 0.7800 0.7460 0.4168 0.049 Uiso 1 1 d R
O12 O 0.5869(2) 0.8955(2) 0.5743(2) 0.0324(7) Uani 1 1 d .
H12A H 0.5223 0.9550 0.5802 0.049 Uiso 1 1 d R
H12B H 0.6606 0.9154 0.5052 0.049 Uiso 1 1 d R
O3 O 0.9518(3) 0.4101(2) 0.7088(2) 0.0320(6) Uani 1 1 d .
O10 O 0.4177(3) 0.5891(2) 0.5630(2) 0.0342(7) Uani 1 1 d .
H10A H 0.3589 0.6164 0.5263 0.051 Uiso 1 1 d R
H10B H 0.3744 0.5484 0.6397 0.051 Uiso 1 1 d R
O9 O 0.9674(3) 0.3672(2) 0.4445(2) 0.0468(8) Uani 1 1 d .
H9A H 1.0503 0.3285 0.4244 0.070 Uiso 1 1 d R
H9B H 0.9759 0.4423 0.4262 0.070 Uiso 1 1 d R
O11 O 0.2951(3) 0.7978(2) 0.6993(2) 0.0385(7) Uani 1 1 d .
H11A H 0.2435 0.7383 0.7373 0.058 Uiso 1 1 d R
H11B H 0.2544 0.8550 0.6567 0.058 Uiso 1 1 d R
N2 N 0.7885(3) 0.0751(3) 0.7544(2) 0.0210(7) Uani 1 1 d .
C13 C 1.0519(4) 0.0770(3) 0.6329(3) 0.0246(9) Uani 1 1 d .
O7 O 0.6963(3) 0.2516(2) 0.5925(3) 0.0371(7) Uani 1 1 d .
C11 C 0.9132(4) 0.3998(3) 0.8269(4) 0.0345(10) Uani 1 1 d .
N1 N 0.6939(3) 0.3160(3) 0.8622(3) 0.0266(8) Uani 1 1 d .
C1 C 0.7804(3) 0.0307(3) 0.8850(3) 0.0222(8) Uani 1 1 d .
C9 C 0.6300(4) 0.5155(3) 0.7225(3) 0.0258(9) Uani 1 1 d .
C12 C 0.9164(3) 0.0281(3) 0.6570(3) 0.0263(9) Uani 1 1 d .
H12C H 0.9031 0.0494 0.5767 0.032 Uiso 1 1 calc R
H12D H 0.9272 -0.0593 0.6854 0.032 Uiso 1 1 calc R
C15 C 0.6313(4) 0.1585(3) 0.6343(3) 0.0240(9) Uani 1 1 d .
C8 C 0.5990(5) 0.4291(4) 0.8513(4) 0.0520(14) Uani 1 1 d .
H8A H 0.5995 0.4717 0.9091 0.062 Uiso 1 1 calc R
H8B H 0.5023 0.4075 0.8832 0.062 Uiso 1 1 calc R
C14 C 0.6593(3) 0.0591(3) 0.7411(3) 0.0240(9) Uani 1 1 d .
H14A H 0.5772 0.0591 0.8220 0.029 Uiso 1 1 calc R
H14B H 0.6714 -0.0184 0.7228 0.029 Uiso 1 1 calc R
C6 C 0.6885(3) 0.0951(3) 0.9766(3) 0.0231(8) Uani 1 1 d .
C5 C 0.6828(4) 0.0516(4) 1.1016(3) 0.0343(10) Uani 1 1 d .
H5 H 0.6220 0.0935 1.1630 0.041 Uiso 1 1 calc R
C7 C 0.6035(4) 0.2140(3) 0.9443(3) 0.0287(9) Uani 1 1 d .
H7A H 0.5488 0.2043 0.8999 0.034 Uiso 1 1 calc R
H7B H 0.5358 0.2345 1.0239 0.034 Uiso 1 1 calc R
C3 C 0.8537(5) -0.1122(4) 1.0483(4) 0.0485(13) Uani 1 1 d .
H3 H 0.9100 -0.1810 1.0717 0.058 Uiso 1 1 calc R
C2 C 0.8622(4) -0.0729(3) 0.9222(4) 0.0371(11) Uani 1 1 d .
H2 H 0.9232 -0.1163 0.8623 0.044 Uiso 1 1 calc R
C4 C 0.7637(5) -0.0509(4) 1.1377(4) 0.0453(12) Uani 1 1 d .
H4 H 0.7570 -0.0781 1.2223 0.054 Uiso 1 1 calc R
C10 C 0.7907(5) 0.3247(4) 0.9197(4) 0.0408(11) Uani 1 1 d .
H10C H 0.8294 0.2439 0.9515 0.049 Uiso 1 1 calc R
H10D H 0.7356 0.3594 0.9929 0.049 Uiso 1 1 calc R
O14 O 0.2085(3) 0.2489(2) 0.2826(2) 0.0599(10) Uani 1 1 d G
H14C H 0.1475 0.3106 0.2838 0.090 Uiso 1 1 d G
H14D H 0.2687 0.2523 0.2056 0.090 Uiso 1 1 d G
O15 O 0.2466(3) 0.3647(3) 0.0295(2) 0.0936(14) Uani 1 1 d G
H15A H 0.1611 0.3968 0.0583 0.140 Uiso 1 1 d G
H15B H 0.2648 0.3493 -0.0415 0.140 Uiso 1 1 d G
O16 O 0.0974(4) 0.6425(3) 0.8566(2) 0.0873(13) Uani 1 1 d G
H16A H 0.0886 0.6095 0.9340 0.131 Uiso 1 1 d G
H16B H 0.0685 0.5973 0.8304 0.131 Uiso 1 1 d G
O17 O 0.3041(3) 0.3858(3) 0.7651(2) 0.137(2) Uani 1 1 d G
H17A H 0.3753 0.3540 0.7854 0.206 Uiso 1 1 d G
H17B H 0.2888 0.3410 0.7290 0.206 Uiso 1 1 d G
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'
Mn Mn 0.3368 0.7283 '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'
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
O9 Mn1 O7 84.92(11) . .
O9 Mn1 O5 83.45(10) . .
O7 Mn1 O5 117.33(10) . .
O9 Mn1 O1 83.33(9) . .
O7 Mn1 O1 81.66(10) . .
O5 Mn1 O1 155.67(10) . .
O9 Mn1 O3 94.68(10) . .
O7 Mn1 O3 162.78(9) . .
O5 Mn1 O3 79.63(10) . .
O1 Mn1 O3 81.19(10) . .
O9 Mn1 N1 158.08(10) . .
O7 Mn1 N1 101.19(11) . .
O5 Mn1 N1 111.36(10) . .
O1 Mn1 N1 76.86(9) . .
O3 Mn1 N1 73.26(10) . .
O2 Mn2 O11 93.40(10) . .
O2 Mn2 O12 94.13(10) . .
O11 Mn2 O12 88.98(10) . .
O2 Mn2 O8 175.96(9) . 2_666
O11 Mn2 O8 89.47(9) . 2_666
O12 Mn2 O8 88.77(10) . 2_666
O2 Mn2 O10 86.97(10) . .
O11 Mn2 O10 89.95(10) . .
O12 Mn2 O10 178.51(9) . .
O8 Mn2 O10 90.19(9) 2_666 .
O2 Mn2 O13 87.41(9) . .
O11 Mn2 O13 177.27(10) . .
O12 Mn2 O13 88.36(10) . .
O8 Mn2 O13 89.85(9) 2_666 .
O10 Mn2 O13 92.70(10) . .
C15 O8 Mn2 127.3(2) . 2_666
C9 O1 Mn1 117.1(2) . .
C9 O2 Mn2 127.1(2) . .
C13 O5 Mn1 120.7(2) . .
C11 O3 Mn1 117.6(3) . .
C1 N2 C12 115.3(3) . .
C1 N2 C14 113.3(3) . .
C12 N2 C14 109.3(3) . .
O6 C13 O5 125.1(4) . .
O6 C13 C12 118.0(3) . .
O5 C13 C12 116.8(3) . .
C15 O7 Mn1 131.6(2) . .
O4 C11 O3 125.0(4) . .
O4 C11 C10 117.3(4) . .
O3 C11 C10 117.7(4) . .
C10 N1 C8 110.0(3) . .
C10 N1 C7 110.3(3) . .
C8 N1 C7 108.7(3) . .
C10 N1 Mn1 105.1(2) . .
C8 N1 Mn1 106.4(2) . .
C7 N1 Mn1 116.2(2) . .
C2 C1 C6 119.1(3) . .
C2 C1 N2 121.9(3) . .
C6 C1 N2 119.0(3) . .
O1 C9 O2 125.0(3) . .
O1 C9 C8 119.6(3) . .
O2 C9 C8 115.3(3) . .
N2 C12 C13 112.6(3) . .
O8 C15 O7 125.0(3) . .
O8 C15 C14 117.6(3) . .
O7 C15 C14 117.5(3) . .
N1 C8 C9 118.7(3) . .
N2 C14 C15 111.5(3) . .
C5 C6 C1 118.2(3) . .
C5 C6 C7 118.2(3) . .
C1 C6 C7 123.5(3) . .
C4 C5 C6 122.4(4) . .
N1 C7 C6 113.7(3) . .
C4 C3 C2 120.6(4) . .
C1 C2 C3 120.6(4) . .
C3 C4 C5 119.2(4) . .
N1 C10 C11 113.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O9 2.184(2) .
Mn1 O7 2.197(3) .
Mn1 O5 2.201(2) .
Mn1 O1 2.228(2) .
Mn1 O3 2.257(3) .
Mn1 N1 2.339(3) .
Mn2 O2 2.159(2) .
Mn2 O11 2.166(2) .
Mn2 O12 2.177(3) .
Mn2 O8 2.197(2) 2_666
Mn2 O10 2.214(3) .
Mn2 O13 2.228(2) .
O8 C15 1.247(4) .
O8 Mn2 2.197(2) 2_666
O1 C9 1.257(4) .
O4 C11 1.250(5) .
O2 C9 1.265(4) .
O6 C13 1.246(4) .
O5 C13 1.260(4) .
O3 C11 1.253(4) .
N2 C1 1.444(4) .
N2 C12 1.470(4) .
N2 C14 1.476(4) .
C13 C12 1.515(5) .
O7 C15 1.258(4) .
C11 C10 1.508(6) .
N1 C10 1.476(5) .
N1 C8 1.477(4) .
N1 C7 1.491(5) .
C1 C2 1.390(5) .
C1 C6 1.403(5) .
C9 C8 1.487(5) .
C15 C14 1.514(5) .
C6 C5 1.389(5) .
C6 C7 1.514(5) .
C5 C4 1.372(5) .
C3 C4 1.359(6) .
C3 C2 1.390(5) .
