#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/52/7005290.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_7005290
loop_
_publ_author_name
'Jordi Gómez-Segura'
'Javier Campo'
'Inhar Imaz'
'Klaus Wurst'
'Jaume Veciana'
'Philippe Gerbier'
'Daniel Ruiz-Molina'
_publ_section_title
;
 New insights into the thermal stability of Mn12 clusters: The case of
 complex [Mn12O12(O2CC?CH)16(H2O)4]?3H2O and its thermolysis derived
 [Mn3(O2CC?CH)6(H2O)4]?2H2O complex
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              2450
_journal_paper_doi               10.1039/b700298j
_journal_year                    2007
_chemical_formula_moiety         'C18 H18 Mn3 O18'
_chemical_formula_sum            'C18 H18 Mn3 O18'
_chemical_formula_weight         687.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.630(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2800(2)
_cell_length_b                   9.4132(2)
_cell_length_c                   14.9675(3)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      1.0
_cell_volume                     1289.05(5)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7142
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         2.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0055(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    'constr, refined at O7, O8 and O9'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0193
_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)+(0.0227P)²+0.6154P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0498
_reflns_number_gt                1889
_reflns_number_total             2057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700298j.txt
_cod_data_source_block           Mn3prop
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7005290
loop_
_symmetry_equiv_pos_as_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_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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.0000 0.0000 0.0000 0.01590(12) Uani 1 2 d S . .
Mn2 Mn 0.19973(3) 0.07377(3) 0.208595(16) 0.01826(11) Uani 1 1 d . . .
O1 O 0.14524(12) 0.16472(12) -0.02529(7) 0.0220(3) Uani 1 1 d . . .
O2 O 0.27911(13) 0.21356(13) 0.11012(8) 0.0256(3) Uani 1 1 d . . .
O3 O 0.17803(12) -0.09183(11) 0.09965(7) 0.0199(3) Uani 1 1 d . . .
O4 O 0.27888(13) -0.25190(12) 0.19868(8) 0.0258(3) Uani 1 1 d . . .
O5 O -0.02176(12) 0.10724(12) 0.12875(7) 0.0209(3) Uani 1 1 d . . .
O6 O -0.12048(14) 0.25958(14) 0.21598(9) 0.0333(3) Uani 1 1 d . . .
O7 O 0.08791(15) -0.05328(13) 0.29658(9) 0.0224(3) Uani 1 1 d . . .
H7A H 0.017(3) -0.101(3) 0.2697(18) 0.059(8) Uiso 1 1 d . . .
H7B H 0.139(3) -0.109(3) 0.3285(18) 0.055(8) Uiso 1 1 d . . .
O8 O 0.42568(15) 0.01783(18) 0.26573(10) 0.0303(3) Uani 1 1 d . . .
H8A H 0.458(3) -0.058(3) 0.2663(17) 0.046(8) Uiso 1 1 d . . .
H85 H 0.490(3) 0.080(3) 0.2703(18) 0.062(9) Uiso 1 1 d . . .
O9 O 0.11291(16) 0.23683(15) -0.20892(10) 0.0307(3) Uani 1 1 d . . .
H9A H 0.130(2) 0.213(2) -0.1571(18) 0.045(7) Uiso 1 1 d . . .
H9B H 0.191(3) 0.233(3) -0.2286(17) 0.055(8) Uiso 1 1 d . . .
C1 C 0.25157(18) 0.22088(17) 0.02520(11) 0.0198(4) Uani 1 1 d . . .
C2 C 0.3531(2) 0.30072(19) -0.02079(12) 0.0267(4) Uani 1 1 d . . .
C3 C 0.4304(2) 0.3606(2) -0.06316(14) 0.0386(5) Uani 1 1 d . . .
H3 H 0.4921 0.4084 -0.0970 0.046 Uiso 1 1 calc . . .
C4 C 0.21471(17) -0.21902(17) 0.12210(11) 0.0181(4) Uani 1 1 d . . .
C5 C 0.1785(2) -0.32682(19) 0.05204(12) 0.0279(4) Uani 1 1 d . . .
C6 C 0.1487(3) -0.4103(2) -0.00655(15) 0.0453(6) Uani 1 1 d . . .
H6 H 0.1248 -0.4771 -0.0534 0.054 Uiso 1 1 calc . . .
C7 C -0.12979(18) 0.16343(19) 0.15948(11) 0.0220(4) Uani 1 1 d . . .
C8 C -0.2741(2) 0.1035(2) 0.12487(12) 0.0299(4) Uani 1 1 d . . .
C9 C -0.3909(2) 0.0539(3) 0.10285(15) 0.0460(6) Uani 1 1 d . . .
H9 H -0.4843 0.0142 0.0852 0.055 Uiso 1 1 calc . . .
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O1 180.00(8) . 3 ?
O1 Mn1 O3 91.10(4) . 3 ?
O1 Mn1 O3 88.90(4) 3 3 ?
O1 Mn1 O3 88.90(4) . . ?
O1 Mn1 O3 91.10(4) 3 . ?
O3 Mn1 O3 180.00(5) 3 . ?
O1 Mn1 O5 91.41(4) . 3 ?
O1 Mn1 O5 88.59(4) 3 3 ?
O3 Mn1 O5 75.97(4) 3 3 ?
O3 Mn1 O5 104.03(4) . 3 ?
O1 Mn1 O5 88.59(4) . . ?
O1 Mn1 O5 91.41(4) 3 . ?
O3 Mn1 O5 104.03(4) 3 . ?
O3 Mn1 O5 75.97(4) . . ?
O5 Mn1 O5 180.00(6) 3 . ?
O4 Mn2 O7 91.78(5) 2 . ?
O4 Mn2 O8 87.26(5) 2 . ?
O7 Mn2 O8 98.88(6) . . ?
O4 Mn2 O2 88.31(4) 2 . ?
O7 Mn2 O2 171.15(5) . . ?
O8 Mn2 O2 89.96(5) . . ?
O4 Mn2 O5 102.57(4) 2 . ?
O7 Mn2 O5 84.90(5) . . ?
O8 Mn2 O5 169.41(5) . . ?
O2 Mn2 O5 86.44(4) . . ?
O4 Mn2 O3 173.87(4) 2 . ?
O7 Mn2 O3 93.70(4) . . ?
O8 Mn2 O3 94.61(5) . . ?
O2 Mn2 O3 85.86(4) . . ?
O5 Mn2 O3 75.20(4) . . ?
C1 O1 Mn1 131.07(10) . . ?
C1 O2 Mn2 132.75(11) . . ?
C4 O3 Mn1 133.04(10) . . ?
C4 O3 Mn2 118.31(10) . . ?
Mn1 O3 Mn2 100.67(4) . . ?
C4 O4 Mn2 140.40(11) . 2_545 ?
C7 O5 Mn1 133.59(10) . . ?
C7 O5 Mn2 124.98(10) . . ?
Mn1 O5 Mn2 101.11(4) . . ?
Mn2 O7 H7A 114.7(17) . . ?
Mn2 O7 H7B 115.4(18) . . ?
H7A O7 H7B 106(2) . . ?
Mn2 O8 H8A 124.9(18) . . ?
Mn2 O8 H85 119.3(18) . . ?
H8A O8 H85 112(2) . . ?
H9A O9 H9B 107(2) . . ?
O1 C1 O2 126.36(15) . . ?
O1 C1 C2 115.86(14) . . ?
O2 C1 C2 117.78(15) . . ?
C3 C2 C1 175.5(2) . . ?
C2 C3 H3 180.0 . . ?
O4 C4 O3 122.98(15) . . ?
O4 C4 C5 120.59(15) . . ?
O3 C4 C5 116.43(14) . . ?
C6 C5 C4 177.8(2) . . ?
C5 C6 H6 180.0 . . ?
O6 C7 O5 125.38(16) . . ?
O6 C7 C8 118.71(15) . . ?
O5 C7 C8 115.89(15) . . ?
C9 C8 C7 175.6(2) . . ?
C8 C9 H9 180.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.1295(11) . ?
Mn1 O1 2.1295(11) 3 ?
Mn1 O3 2.2083(11) 3 ?
Mn1 O3 2.2083(11) . ?
Mn1 O5 2.2144(11) 3 ?
Mn1 O5 2.2144(11) . ?
Mn2 O4 2.1370(11) 2 ?
Mn2 O7 2.1676(12) . ?
Mn2 O8 2.1921(14) . ?
Mn2 O2 2.1931(12) . ?
Mn2 O5 2.2205(11) . ?
Mn2 O3 2.2405(11) . ?
O1 C1 1.255(2) . ?
O2 C1 1.256(2) . ?
O3 C4 1.274(2) . ?
O4 C4 1.239(2) . ?
O4 Mn2 2.1370(11) 2_545 ?
O5 C7 1.285(2) . ?
O6 C7 1.232(2) . ?
O7 H7A 0.84(3) . ?
O7 H7B 0.81(3) . ?
O8 H8A 0.77(3) . ?
O8 H85 0.83(3) . ?
O9 H9A 0.80(3) . ?
O9 H9B 0.83(3) . ?
C1 C2 1.464(2) . ?
C2 C3 1.178(3) . ?
C3 H3 0.9400 . ?
C4 C5 1.458(2) . ?
C5 C6 1.176(3) . ?
C6 H6 0.9400 . ?
C7 C8 1.466(3) . ?
C8 C9 1.176(3) . ?
C9 H9 0.9400 . ?
