#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/63/4306395.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_4306395
loop_
_publ_author_name
'Chen-I Yang'
'Wolfgang Wernsdorfer'
'Kai-Hung Cheng'
'Motohiro Nakano'
'Gene-Hsiang Lee'
'Hui-Lien Tsai'
_publ_section_title
;
A [MnIII3O]7+ Single-Molecule Magnet: the Anisotropy Barrier Enhanced by
Structural Distortion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10184
_journal_page_last               10186
_journal_paper_doi               10.1021/ic8012238
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C55 H46.5 Cl Mn3 N9.5 O11'
_chemical_formula_weight         1216.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.8734(6)
_cell_length_b                   12.8734(6)
_cell_length_c                   18.3364(9)
_cell_measurement_reflns_used    4575
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.22
_cell_volume                     2631.7(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       '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  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20283
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.9365
_exptl_absorpt_correction_T_min  0.7320
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1246
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.390
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4041
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0594P)²+6.9645P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1731
_reflns_number_gt                3623
_reflns_number_total             4041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8012238_si_002.cif
_cod_data_source_block           ic13078
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to
'constr' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C55 H46.50 Cl Mn3 N9.50 O11'
_cod_database_code               4306395
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.50030(5) 0.77031(5) 0.27487(3) 0.01443(18) Uani 1 1 d . . .
O1 O 0.3333 0.6667 0.2602(3) 0.0156(10) Uani 1 3 d S . .
O2 O 0.6604(3) 0.8741(3) 0.29728(16) 0.0202(6) Uani 1 1 d . . .
O3 O 0.5252(2) 0.6363(2) 0.26975(16) 0.0179(6) Uani 1 1 d . . .
N1 N 0.4666(3) 0.9003(3) 0.30049(18) 0.0150(7) Uani 1 1 d . . .
N2 N 0.5468(3) 0.8147(3) 0.15565(19) 0.0207(7) Uani 1 1 d . . .
N3 N 0.5155(5) 0.8531(5) -0.1190(3) 0.0486(13) Uani 1 1 d . . .
C1 C 0.7025(4) 0.9577(3) 0.3487(2) 0.0157(8) Uani 1 1 d . . .
C2 C 0.8205(4) 1.0007(4) 0.3725(2) 0.0201(8) Uani 1 1 d . . .
H2 H 0.8670 0.9704 0.3508 0.024 Uiso 1 1 calc R . .
C3 C 0.8704(4) 1.0855(4) 0.4263(2) 0.0242(9) Uani 1 1 d . . .
H3 H 0.9508 1.1135 0.4413 0.029 Uiso 1 1 calc R . .
C4 C 0.8041(4) 1.1307(4) 0.4592(2) 0.0228(9) Uani 1 1 d . . .
H4 H 0.8372 1.1865 0.4982 0.027 Uiso 1 1 calc R . .
C5 C 0.6899(4) 1.0938(4) 0.4348(2) 0.0204(8) Uani 1 1 d . . .
H5 H 0.6459 1.1271 0.4563 0.024 Uiso 1 1 calc R . .
C6 C 0.6363(4) 1.0085(3) 0.3789(2) 0.0157(8) Uani 1 1 d . . .
C7 C 0.5196(4) 0.9819(3) 0.3505(2) 0.0166(8) Uani 1 1 d . . .
C8 C 0.4606(4) 1.0490(4) 0.3791(3) 0.0248(9) Uani 1 1 d . . .
H8A H 0.5118 1.1348 0.3689 0.037 Uiso 1 1 calc R . .
H8B H 0.4488 1.0366 0.4319 0.037 Uiso 1 1 calc R . .
H8C H 0.3827 1.0195 0.3552 0.037 Uiso 1 1 calc R . .
C9 C 0.6263(4) 0.7911(4) 0.1232(3) 0.0263(10) Uani 1 1 d . . .
H9 H 0.6741 0.7711 0.1531 0.032 Uiso 1 1 calc R . .
C10 C 0.6418(4) 0.7946(4) 0.0489(3) 0.0268(10) Uani 1 1 d . . .
H10 H 0.6988 0.7767 0.0283 0.032 Uiso 1 1 calc R . .
C11 C 0.5736(4) 0.8245(4) 0.0040(2) 0.0237(9) Uani 1 1 d . . .
C12 C 0.4954(4) 0.8543(4) 0.0379(3) 0.0266(10) Uani 1 1 d . . .
H12 H 0.4492 0.8784 0.0097 0.032 Uiso 1 1 calc R . .
C13 C 0.4856(4) 0.8485(4) 0.1121(2) 0.0251(9) Uani 1 1 d . . .
H13 H 0.4320 0.8699 0.1341 0.030 Uiso 1 1 calc R . .
C14 C 0.5235(6) 0.8471(6) -0.1931(3) 0.0436(14) Uani 1 1 d . . .
H14 H 0.4781 0.8695 -0.2235 0.052 Uiso 1 1 calc R . .
C15 C 0.5952(6) 0.8095(6) -0.2241(3) 0.0457(15) Uani 1 1 d . . .
H15 H 0.5999 0.8042 -0.2756 0.055 Uiso 1 1 calc R . .
C16 C 0.6596(8) 0.7800(7) -0.1788(3) 0.063(2) Uani 1 1 d . . .
H16 H 0.7106 0.7543 -0.1995 0.075 Uiso 1 1 calc R . .
C17 C 0.6544(6) 0.7855(6) -0.1061(3) 0.0424(14) Uani 1 1 d . . .
H17 H 0.7011 0.7646 -0.0759 0.051 Uiso 1 1 calc R . .
C18 C 0.5819(5) 0.8210(4) -0.0768(3) 0.0274(10) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.6667 0.43622(9) 0.0147(3) Uani 1 3 d S . .
O4 O 0.3333 0.6667 0.5138(3) 0.0228(11) Uani 1 3 d S . .
O5 O 0.4551(2) 0.7164(3) 0.40977(16) 0.0189(6) Uani 1 1 d . . .
N4 N 0.0000 0.0000 1.0000 0.192(15) Uiso 1 6 d S . .
C19 C 0.0000 0.0000 0.9384(18) 0.092(10) Uiso 0.50 3 d SPD . .
C20 C 0.0000 0.0000 0.8572(19) 0.16(2) Uiso 0.50 3 d SPD . .
H20A H -0.0783 -0.0155 0.8394 0.241 Uiso 0.17 1 calc PR . .
H20B H 0.0155 -0.0627 0.8394 0.241 Uiso 0.17 1 calc PR . .
H20C H 0.0627 0.0783 0.8394 0.241 Uiso 0.17 1 calc PR . .
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'
Cl Cl 0.1484 0.1585 '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
O2 Mn1 O1 175.03(16) . . ?
O2 Mn1 O3 91.95(13) . . ?
O1 Mn1 O3 90.03(9) . . ?
O2 Mn1 N1 88.43(13) . . ?
O1 Mn1 N1 88.73(10) . . ?
O3 Mn1 N1 168.76(13) . . ?
O2 Mn1 N2 88.50(13) . . ?
O1 Mn1 N2 95.98(17) . . ?
O3 Mn1 N2 92.19(13) . . ?
N1 Mn1 N2 99.05(13) . . ?
Mn1 O1 Mn1 118.03(7) 2_665 . ?
Mn1 O1 Mn1 118.03(7) 2_665 3_565 ?
Mn1 O1 Mn1 118.03(7) . 3_565 ?
C1 O2 Mn1 126.8(3) . . ?
N1 O3 Mn1 113.6(2) 3_565 . ?
C7 N1 O3 117.6(3) . 2_665 ?
C7 N1 Mn1 126.8(3) . . ?
O3 N1 Mn1 114.6(2) 2_665 . ?
C13 N2 C9 116.6(4) . . ?
C13 N2 Mn1 122.3(3) . . ?
C9 N2 Mn1 120.3(3) . . ?
C18 N3 C14 118.1(5) . . ?
O2 C1 C2 117.7(4) . . ?
O2 C1 C6 123.7(4) . . ?
C2 C1 C6 118.6(4) . . ?
C3 C2 C1 121.5(4) . . ?
C2 C3 C4 120.3(4) . . ?
C5 C4 C3 119.3(4) . . ?
C4 C5 C6 122.0(4) . . ?
C5 C6 C1 118.1(4) . . ?
C5 C6 C7 119.3(4) . . ?
C1 C6 C7 122.5(4) . . ?
N1 C7 C6 120.3(4) . . ?
N1 C7 C8 119.9(4) . . ?
C6 C7 C8 119.8(4) . . ?
N2 C9 C10 123.1(4) . . ?
C9 C10 C11 119.6(4) . . ?
C12 C11 C10 117.1(4) . . ?
C12 C11 C18 121.8(4) . . ?
C10 C11 C18 121.0(4) . . ?
C13 C12 C11 119.5(4) . . ?
N2 C13 C12 124.0(4) . . ?
C15 C14 N3 121.2(5) . . ?
C16 C15 C14 117.5(5) . . ?
C17 C16 C15 122.8(6) . . ?
C16 C17 C18 118.6(5) . . ?
C17 C18 N3 121.8(5) . . ?
C17 C18 C11 118.8(4) . . ?
N3 C18 C11 119.4(4) . . ?
O4 Cl1 O5 109.56(13) . 2_665 ?
O4 Cl1 O5 109.56(13) . 3_565 ?
O5 Cl1 O5 109.38(13) 2_665 3_565 ?
O4 Cl1 O5 109.56(13) . . ?
O5 Cl1 O5 109.38(13) 2_665 . ?
O5 Cl1 O5 109.38(13) 3_565 . ?
C19 N4 C19 180.00(4) 4_557 . ?
N4 C19 C20 180.00(2) . . ?
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 O2 1.857(3) . ?
Mn1 O1 1.8986(9) . ?
Mn1 O3 1.908(3) . ?
Mn1 N1 1.985(3) . ?
Mn1 N2 2.263(4) . ?
O1 Mn1 1.8986(9) 2_665 ?
O1 Mn1 1.8986(9) 3_565 ?
O2 C1 1.326(5) . ?
O3 N1 1.378(4) 3_565 ?
N1 C7 1.300(5) . ?
N1 O3 1.378(4) 2_665 ?
N2 C13 1.339(6) . ?
N2 C9 1.344(6) . ?
N3 C18 1.360(7) . ?
N3 C14 1.369(7) . ?
C1 C2 1.401(6) . ?
C1 C6 1.420(6) . ?
C2 C3 1.370(6) . ?
C3 C4 1.389(6) . ?
C4 C5 1.374(6) . ?
C5 C6 1.405(6) . ?
C6 C7 1.460(6) . ?
C7 C8 1.502(6) . ?
C9 C10 1.376(7) . ?
C10 C11 1.392(7) . ?
C11 C12 1.390(6) . ?
C11 C18 1.488(6) . ?
C12 C13 1.364(6) . ?
C14 C15 1.362(8) . ?
C15 C16 1.357(8) . ?
C16 C17 1.338(8) . ?
C17 C18 1.340(7) . ?
Cl1 O4 1.423(5) . ?
Cl1 O5 1.449(3) 2_665 ?
Cl1 O5 1.449(3) 3_565 ?
Cl1 O5 1.449(3) . ?
N4 C19 1.13(3) 4_557 ?
N4 C19 1.13(3) . ?
C19 C20 1.489(10) . ?
