#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:03:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179229 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/49/4314901.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_4314901
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         'C27 H18 Cl2 Mn5 N9 O7, 3(C8 H20 N)'
_chemical_formula_sum            'C51 H72 Cl2 Mn5 N12 O13'
_chemical_formula_weight         1406.81
_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                   13.4091(17)
_cell_length_b                   13.4091(17)
_cell_length_c                   61.213(8)
_cell_measurement_reflns_used    3696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.20
_cell_volume                     9532(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            14618
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             4350
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3696
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0768P)²+11.8505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                3504
_reflns_number_total             3696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902298y_si_002_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4314901
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-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'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-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
Mn2 Mn 0.6667 0.3333 0.045314(18) 0.0457(3) Uani 1 3 d S . .
Mn1 Mn 0.50735(5) 0.28464(5) 0.095790(11) 0.04611(18) Uani 1 1 d . . .
Mn3 Mn 0.6667 0.3333 0.14502(2) 0.0559(3) Uani 1 3 d S . .
Cl4 Cl 0.6667 0.3333 0.18647(5) 0.0794(7) Uani 1 3 d S . .
Cl5 Cl 0.6667 0.3333 0.00703(3) 0.0525(4) Uani 1 3 d S . .
O1 O 0.6667 0.3333 0.09699(9) 0.0435(10) Uani 1 3 d S . .
O2 O 0.4667(3) 0.1267(3) 0.09865(5) 0.0496(7) Uani 1 1 d . . .
N3 N 0.5124(3) 0.3188(4) 0.13422(6) 0.0471(8) Uani 1 1 d . . .
O3 O 0.3529(3) 0.2467(3) 0.09579(6) 0.0580(8) Uani 1 1 d . . .
C2 C 0.4446(4) 0.3455(4) 0.14004(8) 0.0502(10) Uani 1 1 d . . .
N1 N 0.5525(3) 0.4499(3) 0.09198(6) 0.0479(8) Uani 1 1 d . . .
N2 N 0.4981(4) 0.2560(4) 0.05732(7) 0.0524(9) Uani 1 1 d . . .
O5 O 0.3763(3) 0.3715(3) 0.14575(6) 0.0647(9) Uani 1 1 d . . .
C001 C 0.7596(4) 0.9903(4) 0.96572(7) 0.0479(9) Uani 1 1 d . . .
H00A H 0.6996 0.9650 0.9547 0.058 Uiso 1 1 calc R . .
H00B H 0.7577 0.9222 0.9716 0.058 Uiso 1 1 calc R . .
N4 N 0.7319(3) 1.0492(3) 0.98403(6) 0.0477(8) Uani 1 1 d . . .
C002 C 0.4894(4) 0.4869(4) 0.08308(7) 0.0506(10) Uani 1 1 d . . .
C003 C 0.3701(4) 0.4123(4) 0.07708(7) 0.0532(10) Uani 1 1 d . . .
O4 O 0.3346(4) 0.0923(5) 0.04454(7) 0.114(2) Uani 1 1 d . . .
C1 C 0.4209(5) 0.1780(5) 0.05145(8) 0.0637(14) Uani 1 1 d . . .
C004 C 0.6463(4) 1.1375(4) 0.95827(9) 0.0585(11) Uani 1 1 d . . .
H00C H 0.6561 1.0978 0.9461 0.088 Uiso 1 1 calc R . .
H00D H 0.6566 1.2102 0.9534 0.088 Uiso 1 1 calc R . .
H00E H 0.5702 1.0918 0.9642 0.088 Uiso 1 1 calc R . .
C005 C 0.3079(4) 0.2972(5) 0.08403(7) 0.0548(11) Uani 1 1 d . . .
C006 C 0.3149(5) 0.4591(5) 0.06514(8) 0.0634(13) Uani 1 1 d . . .
H006 H 0.3566 0.5358 0.0608 0.076 Uiso 1 1 calc R . .
C007 C 0.8755(4) 1.0645(4) 0.95464(8) 0.0544(11) Uani 1 1 d . . .
H00F H 0.8777 1.1312 0.9483 0.082 Uiso 1 1 calc R . .
H00G H 0.8859 1.0208 0.9434 0.082 Uiso 1 1 calc R . .
H00H H 0.9360 1.0884 0.9652 0.082 Uiso 1 1 calc R . .
C008 C 0.1904(5) 0.2326(5) 0.07873(8) 0.0626(12) Uani 1 1 d . . .
H008 H 0.1473 0.1566 0.0834 0.075 Uiso 1 1 calc R . .
C009 C 0.7347(4) 1.1578(4) 0.97578(8) 0.0521(10) Uani 1 1 d . . .
H00I H 0.7225 1.1961 0.9881 0.062 Uiso 1 1 calc R . .
H00J H 0.8109 1.2096 0.9700 0.062 Uiso 1 1 calc R . .
C010 C 0.8199(4) 1.0885(5) 1.00228(8) 0.0604(12) Uani 1 1 d . . .
H01A H 0.7974 1.1240 1.0136 0.072 Uiso 1 1 calc R . .
H01B H 0.8937 1.1472 0.9966 0.072 Uiso 1 1 calc R . .
C011 C 0.5646(4) 1.0035(5) 1.01019(9) 0.0616(12) Uani 1 1 d . . .
H01C H 0.6146 1.0264 1.0227 0.092 Uiso 1 1 calc R . .
H01D H 0.4896 0.9422 1.0142 0.092 Uiso 1 1 calc R . .
H01E H 0.5587 1.0679 1.0050 0.092 Uiso 1 1 calc R . .
C012 C 0.6137(4) 0.9620(4) 0.99215(8) 0.0525(10) Uani 1 1 d . . .
H01F H 0.6165 0.8953 0.9975 0.063 Uiso 1 1 calc R . .
H01G H 0.5609 0.9369 0.9799 0.063 Uiso 1 1 calc R . .
C013 C 0.2001(5) 0.3947(6) 0.05952(9) 0.0680(15) Uani 1 1 d . . .
H013 H 0.1655 0.4269 0.0512 0.082 Uiso 1 1 calc R . .
C014 C 0.1375(5) 0.2822(6) 0.06642(9) 0.0714(16) Uani 1 1 d . . .
H014 H 0.0598 0.2385 0.0629 0.086 Uiso 1 1 calc R . .
C015 C 0.8351(5) 0.9936(7) 1.01261(10) 0.0810(17) Uani 1 1 d . . .
H01H H 0.7613 0.9250 1.0140 0.122 Uiso 1 1 calc R . .
H01I H 0.8693 1.0178 1.0268 0.122 Uiso 1 1 calc R . .
H01J H 0.8842 0.9781 1.0035 0.122 Uiso 1 1 calc R . .
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
N2 Mn2 N2 108.37(13) 2_655 3_665 ?
N2 Mn2 N2 108.37(13) 2_655 . ?
N2 Mn2 N2 108.37(13) 3_665 . ?
N2 Mn2 Cl5 110.55(13) 2_655 . ?
N2 Mn2 Cl5 110.55(13) 3_665 . ?
N2 Mn2 Cl5 110.55(13) . . ?
O3 Mn1 O1 175.66(15) . . ?
O3 Mn1 O2 92.02(13) . . ?
O1 Mn1 O2 91.49(10) . . ?
O3 Mn1 N1 88.95(15) . . ?
O1 Mn1 N1 87.60(11) . . ?
O2 Mn1 N1 178.25(16) . . ?
O3 Mn1 N2 89.69(15) . . ?
O1 Mn1 N2 93.04(19) . . ?
O2 Mn1 N2 87.06(15) . . ?
N1 Mn1 N2 91.49(15) . . ?
O3 Mn1 N3 88.47(14) . . ?
O1 Mn1 N3 88.68(19) . . ?
O2 Mn1 N3 95.02(14) . . ?
N1 Mn1 N3 86.46(15) . . ?
N2 Mn1 N3 177.27(15) . . ?
N3 Mn3 N3 110.44(11) 2_655 3_665 ?
N3 Mn3 N3 110.44(11) 2_655 . ?
N3 Mn3 N3 110.44(11) 3_665 . ?
N3 Mn3 Cl4 108.48(11) 2_655 . ?
N3 Mn3 Cl4 108.48(11) 3_665 . ?
N3 Mn3 Cl4 108.48(11) . . ?
Mn1 O1 Mn1 119.85(2) 2_655 3_665 ?
Mn1 O1 Mn1 119.85(2) 2_655 . ?
Mn1 O1 Mn1 119.85(2) 3_665 . ?
N1 O2 Mn1 114.8(2) 2_655 . ?
C2 N3 Mn3 138.6(4) . . ?
C2 N3 Mn1 113.7(3) . . ?
Mn3 N3 Mn1 105.14(16) . . ?
C005 O3 Mn1 126.0(3) . . ?
O5 C2 N3 179.5(7) . . ?
C002 N1 O2 115.8(4) . 3_665 ?
C002 N1 Mn1 125.4(3) . . ?
O2 N1 Mn1 118.8(3) 3_665 . ?
C1 N2 Mn2 128.7(4) . . ?
C1 N2 Mn1 115.1(4) . . ?
Mn2 N2 Mn1 108.1(2) . . ?
N4 C001 C007 115.0(4) . . ?
C012 N4 C010 111.1(4) . . ?
C012 N4 C001 106.0(3) . . ?
C010 N4 C001 112.0(4) . . ?
C012 N4 C009 111.4(4) . . ?
C010 N4 C009 105.6(4) . . ?
C001 N4 C009 110.9(3) . . ?
N1 C002 C003 123.4(5) . . ?
C006 C003 C005 119.7(5) . . ?
C006 C003 C002 118.4(5) . . ?
C005 C003 C002 121.8(4) . . ?
N2 C1 O4 178.6(6) . . ?
O3 C005 C008 117.9(5) . . ?
O3 C005 C003 123.7(4) . . ?
C008 C005 C003 118.4(5) . . ?
C013 C006 C003 121.8(6) . . ?
C005 C008 C014 120.4(6) . . ?
C004 C009 N4 114.7(4) . . ?
N4 C010 C015 114.9(4) . . ?
N4 C012 C011 115.7(4) . . ?
C014 C013 C006 119.2(5) . . ?
C013 C014 C008 120.4(5) . . ?
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
Mn2 N2 2.093(4) 2_655 ?
Mn2 N2 2.093(4) 3_665 ?
Mn2 N2 2.093(4) . ?
Mn2 Cl5 2.343(2) . ?
Mn1 O3 1.869(3) . ?
Mn1 O1 1.8975(7) . ?
Mn1 O2 1.912(3) . ?
Mn1 N1 1.998(4) . ?
Mn1 N2 2.379(5) . ?
Mn1 N3 2.391(4) . ?
Mn3 N3 2.087(4) 2_655 ?
Mn3 N3 2.087(4) 3_665 ?
Mn3 N3 2.087(4) . ?
Mn3 Cl4 2.537(3) . ?
O1 Mn1 1.8975(7) 2_655 ?
O1 Mn1 1.8975(7) 3_665 ?
O2 N1 1.372(5) 2_655 ?
N3 C2 1.185(6) . ?
O3 C005 1.323(6) . ?
C2 O5 1.185(6) . ?
N1 C002 1.295(6) . ?
N1 O2 1.372(5) 3_665 ?
N2 C1 1.101(7) . ?
C001 N4 1.520(5) . ?
C001 C007 1.523(6) . ?
N4 C012 1.508(6) . ?
N4 C010 1.515(6) . ?
N4 C009 1.525(6) . ?
C002 C003 1.447(7) . ?
C003 C006 1.393(7) . ?
C003 C005 1.404(7) . ?
O4 C1 1.229(8) . ?
C004 C009 1.519(7) . ?
C005 C008 1.404(7) . ?
C006 C013 1.380(8) . ?
C008 C014 1.409(8) . ?
C010 C015 1.524(10) . ?
C011 C012 1.525(7) . ?
C013 C014 1.376(9) . ?
