#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:03:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179229 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/49/4314900.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_4314900
loop_
_publ_author_name
'Patrick L. Feng'
'Casey J. Stephenson'
'Asma Ajmad'
'Gavin Ogawa'
'Enrique del Barco'
'David N. Hendrickson'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of California-San Diego
La Jolla, CA 92093
USA
;
_publ_contact_author_email       dhendrickson@ucsd.edu
_publ_contact_author_name        'David N. Hendrickson'
_publ_section_title
;
 Large Spin-State Changes in Isostructural Cyanate- and Azide-Bridged
 Mn3IIIMn2II Single-Molecule Magnets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1304
_journal_page_last               1306
_journal_paper_doi               10.1021/ic902298y
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C24 H21 Cl2 Mn5 N21 O7, 3(C8 H20 N)'
_chemical_formula_sum            'C48 H81 Cl2 Mn5 N24 O7'
_chemical_formula_weight         1451.91
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.6691(13)
_cell_length_b                   13.6691(13)
_cell_length_c                   60.259(6)
_cell_measurement_reflns_used    4137
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      1.85
_cell_volume                     9750.6(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Ortep-32
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            16687
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.60
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.090
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4137
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.128
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1070P)²+18.6292P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                3652
_reflns_number_total             4137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902298y_si_002_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        9750.7(16)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4314900
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-y, -x, z+1/2'
'-x+y, -x, z'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
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
C1 C 0.8880(5) 0.5909(6) 0.15778(10) 0.0451(14) Uani 1 1 d . . .
H1 H 0.8496 0.5163 0.1636 0.054 Uiso 1 1 calc R . .
C2 C 0.8496(5) 0.6632(7) 0.16366(12) 0.0519(16) Uani 1 1 d . . .
H2 H 0.7879 0.6402 0.1736 0.062 Uiso 1 1 calc R . .
C3 C 0.9046(6) 0.7714(7) 0.15451(11) 0.0506(16) Uani 1 1 d . . .
H3 H 0.8775 0.8217 0.1577 0.061 Uiso 1 1 calc R . .
C4 C 0.9975(6) 0.8073(6) 0.14090(12) 0.0498(15) Uani 1 1 d . G .
H4 H 1.0342 0.8821 0.1352 0.060 Uiso 1 1 calc R . .
C5 C 1.0386(5) 0.7342(5) 0.13537(9) 0.0386(12) Uani 1 1 d . . .
C6 C 0.9814(5) 0.6214(5) 0.14363(8) 0.0356(12) Uani 1 1 d . D .
C7 C 1.0106(5) 0.5358(5) 0.13731(9) 0.0404(13) Uani 1 1 d . . .
C8 C 0.9342(7) 0.4150(6) 0.14334(14) 0.0620(19) Uani 1 1 d . D .
H8A H 0.9662 0.3694 0.1379 0.093 Uiso 1 1 calc R . .
H8B H 0.8598 0.3882 0.1366 0.093 Uiso 1 1 calc R . .
H8C H 0.9263 0.4079 0.1595 0.093 Uiso 1 1 calc R . .
C9 C 0.8901(10) 0.3328(12) 0.08782(16) 0.095(3) Uani 1 1 d . . .
C10 C 0.7804(10) 0.2370(15) 0.0964(2) 0.155(9) Uani 1 1 d . A .
C11 C 0.8397(11) 0.2464(18) 0.0493(2) 0.091(7) Uani 0.63(2) 1 d P A 1
C12 C 0.8157(15) 0.3371(19) 0.0424(2) 0.087(6) Uani 0.63(2) 1 d P A 1
C11A C 0.9742(14) 0.3932(15) 0.0644(3) 0.044(5) Uani 0.37(2) 1 d P A 2
C12A C 0.883(2) 0.402(2) 0.0493(3) 0.062(7) Uani 0.37(2) 1 d P A 2
C13 C 1.0374(10) 0.3691(11) 0.06182(17) 0.097(3) Uani 1 1 d . A 2
C14 C 1.1014(9) 0.3235(9) 0.04241(16) 0.095(4) Uani 1 1 d . A 2
C15 C 0.9170(15) 0.1710(11) 0.0760(2) 0.096(6) Uani 0.70(2) 1 d P A 2
C15A C 1.0421(15) 0.2848(13) 0.0841(2) 0.029(6) Uani 0.30(2) 1 d P A 2
C16 C 1.0154(13) 0.1800(9) 0.0923(2) 0.115(5) Uani 1 1 d . A 2
Cl1 Cl 1.3333 0.6667 0.21110(5) 0.0744(11) Uani 1 3 d S B 2
Cl2 Cl 1.3333 0.6667 0.03079(6) 0.0727(11) Uani 1 3 d S C 2
Mn1 Mn 1.23359(7) 0.72528(7) 0.122625(12) 0.0337(2) Uani 1 1 d . . 2
Mn2 Mn 1.3333 0.6667 0.17234(2) 0.0361(3) Uani 1 3 d S . 2
Mn3 Mn 1.3333 0.6667 0.07002(2) 0.0382(4) Uani 1 3 d S . 2
N7 N 1.1070(4) 0.5672(4) 0.12684(8) 0.0385(11) Uani 1 1 d . D 2
N4 N 1.2512(4) 0.7520(4) 0.16149(9) 0.0348(11) Uani 1 1 d . E 2
N5 N 1.2502(5) 0.8311(5) 0.16859(8) 0.0447(12) Uani 1 1 d . E 2
N6 N 1.2470(7) 0.9085(6) 0.17581(10) 0.0660(19) Uani 1 1 d . E 2
N1 N 1.2084(5) 0.6932(5) 0.08412(8) 0.0448(12) Uani 1 1 d . F 2
N2 N 1.1154(6) 0.6603(5) 0.07784(9) 0.0517(14) Uani 1 1 d . F 2
N3 N 1.0238(6) 0.6308(7) 0.07214(13) 0.079(2) Uani 1 1 d . F 2
N8 N 0.9364(7) 0.2776(5) 0.06771(10) 0.081(2) Uani 1 1 d . A 2
O1 O 1.3333 0.6667 0.12400(11) 0.0295(13) Uani 1 3 d S . 2
O2 O 1.1274(4) 0.7733(4) 0.12158(7) 0.0430(9) Uani 1 1 d . G 2
O3 O 1.1225(3) 0.4818(3) 0.11896(6) 0.0375(9) Uani 1 1 d . D 2
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'
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'
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
_geom_angle_publ_flag
C2 C1 C6 123.7(6) . . ?
C2 C1 H1 118.1 . . ?
C6 C1 H1 118.1 . . ?
C1 C2 C3 117.6(6) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C4 C3 C2 121.6(7) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 120.7(7) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
O2 C5 C4 117.7(6) . . ?
O2 C5 C6 123.1(5) . . ?
C4 C5 C6 119.1(5) . . ?
C5 C6 C1 117.2(6) . . ?
C5 C6 C7 123.5(5) . . ?
C1 C6 C7 119.2(5) . . ?
N7 C7 C6 119.3(5) . . ?
N7 C7 C8 120.5(6) . . ?
C6 C7 C8 120.1(6) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N8 106.6(12) . . ?
C10 C9 C11A 145.3(11) . . ?
N8 C9 C11A 48.2(7) . . ?
C13 C11A N8 65.0(12) . . ?
C13 C11A C12A 135.7(17) . . ?
N8 C11A C12A 107.5(14) . . ?
C13 C11A C9 114.1(15) . . ?
N8 C11A C9 64.5(9) . . ?
C12A C11A C9 98.2(13) . . ?
C11A C13 N8 69.3(13) . . ?
C11A C13 C14 145.4(13) . . ?
N8 C13 C14 107.7(9) . . ?
C11A C13 C15A 112.5(14) . . ?
N8 C13 C15A 64.0(8) . . ?
C14 C13 C15A 95.0(10) . . ?
N8 C15 C16 114.1(10) . . ?
N8 C15 C15A 65.3(8) . . ?
C16 C15 C15A 48.9(8) . . ?
C16 C15A N8 111.6(11) . . ?
C16 C15A C15 62.1(10) . . ?
N8 C15A C15 49.6(8) . . ?
C16 C15A C13 149.2(12) . . ?
N8 C15A C13 45.9(6) . . ?
C15 C15A C13 91.7(10) . . ?
C15A C16 C15 69.0(10) . . ?
O2 Mn1 O1 176.21(15) . . ?
O2 Mn1 O3 92.64(19) . 4_775 ?
O1 Mn1 O3 91.15(12) . 4_775 ?
O2 Mn1 N7 88.8(2) . . ?
O1 Mn1 N7 87.40(15) . . ?
O3 Mn1 N7 178.38(19) 4_775 . ?
O2 Mn1 N1 88.02(19) . . ?
O1 Mn1 N1 91.9(2) . . ?
O3 Mn1 N1 93.2(2) 4_775 . ?
N7 Mn1 N1 87.5(2) . . ?
O2 Mn1 N4 90.93(18) . . ?
O1 Mn1 N4 89.0(2) . . ?
O3 Mn1 N4 88.85(17) 4_775 . ?
N7 Mn1 N4 90.42(18) . . ?
N1 Mn1 N4 177.7(2) . . ?
N4 Mn2 N4 110.66(14) . 2_755 ?
N4 Mn2 N4 110.66(14) . 4_775 ?
N4 Mn2 N4 110.66(14) 2_755 4_775 ?
N4 Mn2 Cl1 108.25(15) . . ?
N4 Mn2 Cl1 108.25(15) 2_755 . ?
N4 Mn2 Cl1 108.25(15) 4_775 . ?
N1 Mn3 N1 104.66(17) . 4_775 ?
N1 Mn3 N1 104.66(17) . 2_755 ?
N1 Mn3 N1 104.66(17) 4_775 2_755 ?
N1 Mn3 Cl2 113.94(15) . . ?
N1 Mn3 Cl2 113.94(15) 4_775 . ?
N1 Mn3 Cl2 113.94(15) 2_755 . ?
C7 N7 O3 116.2(5) . . ?
C7 N7 Mn1 126.5(4) . . ?
O3 N7 Mn1 117.2(4) . . ?
N5 N4 Mn2 131.3(5) . . ?
N5 N4 Mn1 117.2(4) . . ?
Mn2 N4 Mn1 105.4(2) . . ?
N6 N5 N4 178.5(8) . . ?
N2 N1 Mn3 128.3(5) . . ?
N2 N1 Mn1 114.6(4) . . ?
Mn3 N1 Mn1 112.1(2) . . ?
N3 N2 N1 177.5(8) . . ?
C13 N8 C11A 45.7(8) . . ?
C13 N8 C15 127.5(12) . . ?
C11A N8 C15 165.1(10) . . ?
C13 N8 C9 102.0(8) . . ?
C11A N8 C9 67.4(9) . . ?
C15 N8 C9 106.3(8) . . ?
C13 N8 C15A 70.1(8) . . ?
C11A N8 C15A 101.1(9) . . ?
C15 N8 C15A 65.1(10) . . ?
C9 N8 C15A 93.1(7) . . ?
Mn1 O1 Mn1 119.81(3) . 4_775 ?
Mn1 O1 Mn1 119.81(3) . 2_755 ?
Mn1 O1 Mn1 119.81(3) 4_775 2_755 ?
C5 O2 Mn1 123.0(4) . . ?
N7 O3 Mn1 114.2(3) . 2_755 ?
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
C1 C2 1.376(10) . ?
C1 C6 1.414(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.395(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.410(9) . ?
C4 H4 0.9500 . ?
C5 O2 1.342(7) . ?
C5 C6 1.424(8) . ?
C6 C7 1.464(9) . ?
C7 N7 1.323(8) . ?
C7 C8 1.492(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.504(16) . ?
C9 N8 1.708(13) . ?
C9 C11A 1.75(2) . ?
C11 C12 1.49(3) . ?
C11A C13 1.079(18) . ?
C11A N8 1.41(2) . ?
C11A C12A 1.59(3) . ?
C13 N8 1.367(12) . ?
C13 C14 1.751(19) . ?
C13 C15A 1.792(19) . ?
C15 N8 1.435(17) . ?
C15 C16 1.62(2) . ?
C15 C15A 1.71(2) . ?
C15A C16 1.380(19) . ?
C15A N8 1.712(18) . ?
Cl1 Mn2 2.335(3) . ?
Cl2 Mn3 2.363(4) . ?
Mn1 O2 1.869(4) . ?
Mn1 O1 1.8974(10) . ?
Mn1 O3 1.938(4) 4_775 ?
Mn1 N7 1.997(5) . ?
Mn1 N1 2.354(5) . ?
Mn1 N4 2.364(5) . ?
Mn2 N4 2.087(5) . ?
Mn2 N4 2.087(5) 2_755 ?
Mn2 N4 2.087(5) 4_775 ?
Mn3 N1 2.095(6) . ?
Mn3 N1 2.095(6) 4_775 ?
Mn3 N1 2.095(5) 2_755 ?
N7 O3 1.372(6) . ?
N4 N5 1.169(8) . ?
N5 N6 1.165(8) . ?
N1 N2 1.178(8) . ?
N2 N3 1.160(9) . ?
O1 Mn1 1.8974(10) 4_775 ?
O1 Mn1 1.8974(10) 2_755 ?
O3 Mn1 1.938(4) 2_755 ?
