#------------------------------------------------------------------------------
#$Date: 2017-12-11 01:28:22 +0200 (Mon, 11 Dec 2017) $
#$Revision: 204147 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/48/4314899.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_4314899
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         'C21 H12 Br2 Mn5 N21 O7, 3(C8 H20 N)'
_chemical_formula_sum            'C45 H75 Br2 Mn5 N24 O7'
_chemical_formula_weight         1498.73
_space_group.centring_type       P
_space_group_IT_number           161
_space_group.IT_number           161
_symmetry_cell_setting           hexagonal
_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                   13.481(5)
_cell_length_b                   13.481(5)
_cell_length_c                   60.88(2)
_cell_measurement_reflns_used    4079
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      1.87
_cell_volume                     9582(6)
_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 0.992
_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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_refln_scan_rate          10
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            40270
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.77
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.277
_exptl_absorpt_correction_T_max  0.9776
_exptl_absorpt_correction_T_min  0.9144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4584
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'flack h d (1983), acta cryst. a39, 876-881'
_refine_ls_abs_structure_Flack   0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4079
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(fo²)+(0.0438p)²+0.0000p] where p=(fo²+2fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                3707
_reflns_number_total             4079
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ic902298y_si_002_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_structure_factor_coef' value 'fsqd' changed to 'Fsqd'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_atom_site_adp_type'
value 'uani' changed to 'Uani' according to the built-in table from
CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29 (31 time).

'_atom_site_adp_type' value 'uiso' changed to
'Uiso' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (25
times).

'_atom_site_refinement_flags' value 'r' changed to 'R'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (25
times).

'_atom_site_refinement_flags' value 's' changed to 'S'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_space_group.centring_type' value 'primitive' was replaced with the
value 'P' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_original_cell_volume        9583(6)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4314899
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 -0.3228(2) -0.3553(2) 0.21796(4) 0.0303(5) Uani 1 1 d . . .
c2 c -0.3756(2) -0.4708(2) 0.22337(5) 0.0369(6) Uani 1 1 d . . .
h2 h -0.3432 -0.5152 0.2184 0.044 Uiso 1 1 calc R . .
c3 c -0.4754(3) -0.5225(3) 0.23596(5) 0.0403(7) Uani 1 1 d . . .
h3 h -0.5102 -0.6016 0.2395 0.048 Uiso 1 1 calc R . .
c4 c -0.5241(2) -0.4590(3) 0.24334(5) 0.0401(7) Uani 1 1 d . . .
h4 h -0.5916 -0.4943 0.2520 0.048 Uiso 1 1 calc R . .
c5 c -0.4744(2) -0.3451(2) 0.23799(5) 0.0353(6) Uani 1 1 d . . .
h5 h -0.5084 -0.3021 0.2429 0.042 Uiso 1 1 calc R . .
c6 c -0.3732(2) -0.2909(2) 0.22522(4) 0.0308(5) Uani 1 1 d . . .
c7 c -0.3279(2) -0.1723(2) 0.21913(4) 0.0284(5) Uani 1 1 d . . .
h7 h -0.3734 -0.1382 0.2220 0.034 Uiso 1 1 calc R . .
c8 c 0.5706(2) 0.8939(2) 0.17090(5) 0.0350(6) Uani 1 1 d . . .
h8a h 0.5731 0.8270 0.1649 0.042 Uiso 1 1 calc R . .
h8b h 0.6310 0.9290 0.1823 0.042 Uiso 1 1 calc R . .
c9 c 0.4556(3) 0.8518(3) 0.18180(5) 0.0409(6) Uani 1 1 d . . .
h9a h 0.4448 0.7964 0.1933 0.061 Uiso 1 1 calc R . .
h9b h 0.3947 0.8149 0.1708 0.061 Uiso 1 1 calc R . .
h9c h 0.4528 0.9168 0.1883 0.061 Uiso 1 1 calc R . .
c10 c 0.7172(2) 1.0118(3) 0.14432(5) 0.0370(6) Uani 1 1 d . . .
h10a h 0.7710 1.0412 0.1569 0.044 Uiso 1 1 calc R . .
h10b h 0.7148 0.9412 0.1390 0.044 Uiso 1 1 calc R . .
c11 c 0.7641(3) 1.1002(3) 0.12608(6) 0.0476(7) Uani 1 1 d . . .
h11a h 0.8403 1.1146 0.1218 0.071 Uiso 1 1 calc R . .
h11b h 0.7696 1.1716 0.1312 0.071 Uiso 1 1 calc R . .
h11c h 0.7127 1.0714 0.1134 0.071 Uiso 1 1 calc R . .
c12 c 0.5118(2) 0.9317(3) 0.13412(5) 0.0419(6) Uani 1 1 d . . .
h12a h 0.4363 0.9141 0.1400 0.050 Uiso 1 1 calc R . .
h12b h 0.5336 0.9912 0.1227 0.050 Uiso 1 1 calc R . .
c13 c 0.4994(3) 0.8247(4) 0.12344(6) 0.0574(9) Uani 1 1 d . . .
h13a h 0.4411 0.7990 0.1119 0.086 Uiso 1 1 calc R . .
h13b h 0.4761 0.7643 0.1345 0.086 Uiso 1 1 calc R . .
h13c h 0.5728 0.8415 0.1170 0.086 Uiso 1 1 calc R . .
c14 c 0.5958(2) 1.0850(2) 0.16097(5) 0.0386(6) Uani 1 1 d . . .
h14a h 0.6064 1.1358 0.1484 0.046 Uiso 1 1 calc R . .
h14b h 0.5189 1.0596 0.1672 0.046 Uiso 1 1 calc R . .
c15 c 0.6843(3) 1.1539(3) 0.17819(5) 0.0417(7) Uani 1 1 d . . .
h15a h 0.6754 1.2187 0.1827 0.063 Uiso 1 1 calc R . .
h15b h 0.7611 1.1824 0.1721 0.063 Uiso 1 1 calc R . .
h15c h 0.6739 1.1052 0.1909 0.063 Uiso 1 1 calc R . .
mn2 mn 0.0000 0.0000 0.255684(12) 0.03001(17) Uani 1 3 d S . .
n7 n -0.22969(19) -0.11062(17) 0.21009(4) 0.0274(4) Uani 1 1 d . . .
n8 n 0.59873(19) 0.9806(2) 0.15253(4) 0.0334(5) Uani 1 1 d . . .
o1 o 0.0000 0.0000 0.20469(6) 0.0250(6) Uani 1 3 d S . .
o2 o -0.22910(15) -0.31047(14) 0.20557(3) 0.0305(4) Uani 1 1 d . . .
o3 o 0.00377(16) -0.20181(14) 0.20311(3) 0.0288(4) Uani 1 1 d . . .
br1 br 0.0000 0.0000 0.115416(7) 0.03332(12) Uani 1 3 d S . .
br2 br 0.0000 0.0000 0.296020(7) 0.03661(12) Uani 1 3 d S . .
mn1 mn -0.11195(3) -0.15801(3) 0.205663(8) 0.02498(9) Uani 1 1 d . . .
mn3 mn 0.0000 0.0000 0.155935(11) 0.02366(15) Uani 1 3 d S . .
n1 n -0.13611(19) -0.15239(18) 0.16809(4) 0.0278(4) Uani 1 1 d . . .
n2 n -0.22929(19) -0.21719(18) 0.16105(3) 0.0290(5) Uani 1 1 d . . .
n3 n -0.3191(2) -0.2814(2) 0.15477(4) 0.0419(6) Uani 1 1 d . . .
n4 n -0.0947(2) -0.1646(2) 0.24329(4) 0.0328(5) Uani 1 1 d . . .
n5 n -0.0912(2) -0.24260(19) 0.25012(3) 0.0330(5) Uani 1 1 d . . .
n6 n -0.0881(4) -0.3244(3) 0.25636(5) 0.0744(11) Uani 1 1 d . . .
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'
br br -0.2901 2.4595 '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
o2 c1 c2 118.8(2) . . ?
o2 c1 c6 122.5(2) . . ?
c2 c1 c6 118.7(2) . . ?
c1 c2 c3 121.1(3) . . ?
c1 c2 h2 119.5 . . ?
c3 c2 h2 119.5 . . ?
c4 c3 c2 120.3(3) . . ?
c4 c3 h3 119.8 . . ?
c2 c3 h3 119.8 . . ?
c5 c4 c3 119.7(3) . . ?
c5 c4 h4 120.1 . . ?
c3 c4 h4 120.1 . . ?
c4 c5 c6 120.9(3) . . ?
c4 c5 h5 119.5 . . ?
c6 c5 h5 119.5 . . ?
c1 c6 c5 119.3(2) . . ?
c1 c6 c7 122.1(2) . . ?
c5 c6 c7 118.6(2) . . ?
n7 c7 c6 123.8(2) . . ?
n7 c7 h7 118.1 . . ?
c6 c7 h7 118.1 . . ?
c9 c8 n8 115.2(2) . . ?
c9 c8 h8a 108.5 . . ?
n8 c8 h8a 108.5 . . ?
c9 c8 h8b 108.5 . . ?
n8 c8 h8b 108.5 . . ?
h8a c8 h8b 107.5 . . ?
c8 c9 h9a 109.5 . . ?
c8 c9 h9b 109.5 . . ?
h9a c9 h9b 109.5 . . ?
c8 c9 h9c 109.5 . . ?
h9a c9 h9c 109.5 . . ?
h9b c9 h9c 109.5 . . ?
c11 c10 n8 115.3(2) . . ?
c11 c10 h10a 108.5 . . ?
n8 c10 h10a 108.5 . . ?
c11 c10 h10b 108.5 . . ?
n8 c10 h10b 108.5 . . ?
h10a c10 h10b 107.5 . . ?
c10 c11 h11a 109.5 . . ?
c10 c11 h11b 109.5 . . ?
h11a c11 h11b 109.5 . . ?
c10 c11 h11c 109.5 . . ?
h11a c11 h11c 109.5 . . ?
h11b c11 h11c 109.5 . . ?
c13 c12 n8 115.2(2) . . ?
c13 c12 h12a 108.5 . . ?
n8 c12 h12a 108.5 . . ?
c13 c12 h12b 108.5 . . ?
n8 c12 h12b 108.5 . . ?
h12a c12 h12b 107.5 . . ?
c12 c13 h13a 109.5 . . ?
c12 c13 h13b 109.5 . . ?
h13a c13 h13b 109.5 . . ?
c12 c13 h13c 109.5 . . ?
h13a c13 h13c 109.5 . . ?
h13b c13 h13c 109.5 . . ?
c15 c14 n8 115.2(2) . . ?
c15 c14 h14a 108.5 . . ?
n8 c14 h14a 108.5 . . ?
c15 c14 h14b 108.5 . . ?
n8 c14 h14b 108.5 . . ?
h14a c14 h14b 107.5 . . ?
c14 c15 h15a 109.5 . . ?
c14 c15 h15b 109.5 . . ?
h15a c15 h15b 109.5 . . ?
c14 c15 h15c 109.5 . . ?
h15a c15 h15c 109.5 . . ?
h15b c15 h15c 109.5 . . ?
n4 mn2 n4 107.52(8) . 2 ?
n4 mn2 n4 107.52(8) . 4 ?
n4 mn2 n4 107.52(8) 2 4 ?
n4 mn2 br2 111.36(7) . . ?
n4 mn2 br2 111.36(7) 2 . ?
n4 mn2 br2 111.36(7) 4 . ?
c7 n7 o3 116.0(2) . 4 ?
c7 n7 mn1 125.15(18) . . ?
o3 n7 mn1 118.83(15) 4 . ?
c12 n8 c10 110.8(2) . . ?
c12 n8 c14 106.3(2) . . ?
c10 n8 c14 111.5(2) . . ?
c12 n8 c8 111.6(2) . . ?
c10 n8 c8 106.2(2) . . ?
c14 n8 c8 110.6(2) . . ?
mn1 o1 mn1 119.903(14) 2 . ?
mn1 o1 mn1 119.903(14) 2 4 ?
mn1 o1 mn1 119.903(14) . 4 ?
c1 o2 mn1 126.05(15) . . ?
n7 o3 mn1 113.94(13) 2 . ?
o2 mn1 o1 175.83(9) . . ?
o2 mn1 o3 91.79(7) . . ?
o1 mn1 o3 91.72(6) . . ?
o2 mn1 n7 89.00(8) . . ?
o1 mn1 n7 87.62(6) . . ?
o3 mn1 n7 176.79(9) . . ?
o2 mn1 n4 90.38(8) . . ?
o1 mn1 n4 92.03(13) . . ?
o3 mn1 n4 87.45(8) . . ?
n7 mn1 n4 89.43(9) . . ?
o2 mn1 n1 88.72(7) . . ?
o1 mn1 n1 88.76(13) . . ?
o3 mn1 n1 94.53(8) . . ?
n7 mn1 n1 88.60(9) . . ?
n4 mn1 n1 177.85(10) . . ?
n1 mn3 n1 108.17(7) 2 4 ?
n1 mn3 n1 108.17(7) 2 . ?
n1 mn3 n1 108.17(7) 4 . ?
n1 mn3 br1 110.74(6) 2 . ?
n1 mn3 br1 110.74(6) 4 . ?
n1 mn3 br1 110.74(6) . . ?
n2 n1 mn3 132.62(18) . . ?
n2 n1 mn1 116.36(16) . . ?
mn3 n1 mn1 108.25(9) . . ?
n3 n2 n1 178.1(3) . . ?
n5 n4 mn2 124.1(2) . . ?
n5 n4 mn1 116.32(19) . . ?
mn2 n4 mn1 109.88(11) . . ?
n4 n5 n6 177.6(3) . . ?
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 o2 1.329(3) . ?
c1 c2 1.390(4) . ?
c1 c6 1.414(4) . ?
c2 c3 1.394(4) . ?
c2 h2 0.9500 . ?
c3 c4 1.389(5) . ?
c3 h3 0.9500 . ?
c4 c5 1.372(4) . ?
c4 h4 0.9500 . ?
c5 c6 1.415(4) . ?
c5 h5 0.9500 . ?
c6 c7 1.445(4) . ?
c7 n7 1.283(3) . ?
c7 h7 0.9500 . ?
c8 c9 1.512(4) . ?
c8 n8 1.522(3) . ?
c8 h8a 0.9900 . ?
c8 h8b 0.9900 . ?
c9 h9a 0.9800 . ?
c9 h9b 0.9800 . ?
c9 h9c 0.9800 . ?
c10 c11 1.516(4) . ?
c10 n8 1.518(3) . ?
c10 h10a 0.9900 . ?
c10 h10b 0.9900 . ?
c11 h11a 0.9800 . ?
c11 h11b 0.9800 . ?
c11 h11c 0.9800 . ?
c12 c13 1.513(5) . ?
c12 n8 1.514(4) . ?
c12 h12a 0.9900 . ?
c12 h12b 0.9900 . ?
c13 h13a 0.9800 . ?
c13 h13b 0.9800 . ?
c13 h13c 0.9800 . ?
c14 c15 1.509(4) . ?
c14 n8 1.518(4) . ?
c14 h14a 0.9900 . ?
c14 h14b 0.9900 . ?
c15 h15a 0.9800 . ?
c15 h15b 0.9800 . ?
c15 h15c 0.9800 . ?
mn2 n4 2.071(2) . ?
mn2 n4 2.071(2) 2 ?
mn2 n4 2.071(2) 4 ?
mn2 br2 2.4557(12) . ?
n7 o3 1.376(3) 4 ?
n7 mn1 2.004(2) . ?
o1 mn1 1.8984(8) 2 ?
o1 mn1 1.8984(8) . ?
o1 mn1 1.8984(8) 4 ?
o2 mn1 1.8636(18) . ?
o3 n7 1.376(3) 2 ?
o3 mn1 1.9307(19) . ?
br1 mn3 2.4669(11) . ?
mn1 n4 2.309(3) . ?
mn1 n1 2.317(2) . ?
mn3 n1 2.089(2) 2 ?
mn3 n1 2.089(2) 4 ?
mn3 n1 2.089(2) . ?
n1 n2 1.195(3) . ?
n2 n3 1.146(3) . ?
n4 n5 1.153(3) . ?
n5 n6 1.187(4) . ?
