#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:09:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179014 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/12/4121290.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_4121290
loop_
_publ_author_name
'Gang Wu'
'Jiaquan Bai'
'Yuan Jiang'
'Guanghua Li'
'Jian Huang'
'Yi Li'
'Christopher E. Anson'
'Annie K. Powell'
'Shilun Qiu'
_publ_section_title
;
 Rolling Up the Sheet: Constructing Metal-Organic Lamellae and Nanotubes
 from a [{Mn3(propanediolato)2}(dicyanamide)2]n Honeycomb Skeleton
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18276
_journal_page_last               18279
_journal_paper_doi               10.1021/ja409569q
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C32 H54 Br2 Mn3 N9 O12 S2'
_chemical_formula_weight         1145.60
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.254(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4963(11)
_cell_length_b                   11.5794(7)
_cell_length_c                   24.7985(14)
_cell_measurement_reflns_used    5874
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      24.0335
_cell_measurement_theta_min      2.2826
_cell_volume                     5124.1(5)
_computing_cell_refinement       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_collection       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'Apex2 (Bruker AXS Inc., 2005)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25732
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.097
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.427
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9321
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0840P)²+4.2534P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6200
_reflns_number_total             9321
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja409569q_si_003.cif
_cod_data_source_block           sheet_tube_2
_cod_database_code               4121290
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.683
_shelx_estimated_absorpt_t_max   0.743
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.30204(5) 0.52239(7) 0.57921(3) 0.0476(2) Uani 1 1 d . . . . .
Mn2 Mn 0.30679(4) 0.49837(6) 0.70713(3) 0.03391(19) Uani 1 1 d . . . . .
Mn3 Mn 0.30122(5) 0.48445(7) 0.83367(3) 0.0439(2) Uani 1 1 d . . . . .
Br1 Br 0.44037(3) 0.38254(5) 0.72935(2) 0.06015(19) Uani 1 1 d D . . . .
Br2 Br 0.14033(4) 0.63437(5) 0.67448(2) 0.06197(19) Uani 1 1 d . . . . .
O1 O 0.33157(19) 0.6093(3) 0.65938(13) 0.0404(8) Uani 1 1 d . . . . .
C1 C 0.3834(3) 0.6992(4) 0.6783(2) 0.0473(13) Uani 1 1 d . . . . .
H1A H 0.3793 0.7559 0.6477 0.057 Uiso 1 1 calc R U . . .
H1B H 0.4348 0.6670 0.6877 0.057 Uiso 1 1 calc R U . . .
O2 O 0.33218(19) 0.5906(3) 0.77198(12) 0.0397(8) Uani 1 1 d . . . . .
C2 C 0.3847(3) 0.6830(4) 0.7800(2) 0.0532(14) Uani 1 1 d . . . . .
H2A H 0.4361 0.6511 0.7879 0.064 Uiso 1 1 calc R U . . .
H2B H 0.3811 0.7293 0.8128 0.064 Uiso 1 1 calc R U . . .
C3 C 0.3706(3) 0.7603(4) 0.7291(2) 0.0518(14) Uani 1 1 d . . . . .
H3A H 0.4081 0.8244 0.7384 0.062 Uiso 1 1 calc R U . . .
N1 N 0.2986(3) 0.8118(4) 0.7182(2) 0.0609(13) Uani 1 1 d D . . . .
H1 H 0.262(3) 0.782(5) 0.695(2) 0.073 Uiso 1 1 d D U . . .
S1 S 0.28951(12) 0.95011(13) 0.71461(8) 0.0753(5) Uani 1 1 d . . . . .
O5 O 0.2112(3) 0.9708(4) 0.7025(3) 0.108(2) Uani 1 1 d . . . . .
O6 O 0.3366(3) 1.0004(3) 0.7642(2) 0.0930(17) Uani 1 1 d . . . . .
C4 C 0.3212(4) 0.9991(5) 0.6581(3) 0.0613(16) Uani 1 1 d . . . . .
C5 C 0.2785(4) 0.9863(6) 0.6059(4) 0.089(2) Uani 1 1 d . . . . .
H5A H 0.2306 0.9511 0.5995 0.107 Uiso 1 1 calc R U . . .
C6 C 0.3038(4) 1.0244(7) 0.5607(3) 0.089(2) Uani 1 1 d . . . . .
H6A H 0.2732 1.0148 0.5236 0.106 Uiso 1 1 calc R U . . .
C7 C 0.3734(4) 1.0763(6) 0.5696(3) 0.0701(17) Uani 1 1 d . . . . .
C8 C 0.4150(4) 1.0871(7) 0.6232(3) 0.080(2) Uani 1 1 d . . . . .
H8A H 0.4632 1.1215 0.6304 0.096 Uiso 1 1 calc R U . . .
C9 C 0.3894(4) 1.0496(6) 0.6676(3) 0.0686(17) Uani 1 1 d . . . . .
H9A H 0.4195 1.0592 0.7047 0.082 Uiso 1 1 calc R U . . .
C10 C 0.4005(5) 1.1209(8) 0.5209(3) 0.108(3) Uani 1 1 d . . . . .
H10A H 0.3632 1.1032 0.4858 0.162 Uiso 1 1 calc R U . . .
H10B H 0.4482 1.0838 0.5211 0.162 Uiso 1 1 calc R U . . .
H10C H 0.4077 1.2047 0.5244 0.162 Uiso 1 1 calc R U . . .
O3 O 0.26495(18) 0.4193(3) 0.63961(12) 0.0358(7) Uani 1 1 d . . . . .
C11 C 0.2458(3) 0.3010(4) 0.63736(19) 0.0419(12) Uani 1 1 d . . . . .
H11A H 0.2922 0.2543 0.6444 0.050 Uiso 1 1 calc R U . . .
H11B H 0.2149 0.2823 0.5993 0.050 Uiso 1 1 calc R U . . .
O4 O 0.26637(18) 0.4004(3) 0.75275(12) 0.0374(7) Uani 1 1 d . . . . .
C12 C 0.2494(3) 0.2834(4) 0.7397(2) 0.0481(13) Uani 1 1 d . . . . .
H12A H 0.2211 0.2520 0.7652 0.058 Uiso 1 1 calc R U . . .
H12B H 0.2966 0.2391 0.7456 0.058 Uiso 1 1 calc R U . . .
C13 C 0.2032(3) 0.2683(4) 0.67937(19) 0.0458(13) Uani 1 1 d . . . . .
H13A H 0.1899 0.1847 0.6738 0.055 Uiso 1 1 calc R U . . .
N2 N 0.1342(3) 0.3322(4) 0.67182(19) 0.0571(12) Uani 1 1 d D . . . .
H2 H 0.136(3) 0.405(3) 0.671(2) 0.069 Uiso 1 1 d D U . . .
S2 S 0.05483(10) 0.27494(19) 0.64184(7) 0.0805(6) Uani 1 1 d . . . . .
O7 O 0.0498(3) 0.1682(5) 0.6663(3) 0.115(2) Uani 1 1 d . . . . .
O8 O -0.0008(3) 0.3611(6) 0.6407(2) 0.115(2) Uani 1 1 d . . . . .
C14 C 0.0545(4) 0.2448(7) 0.5727(3) 0.078(2) Uani 1 1 d . . . . .
C15 C 0.0428(6) 0.3317(10) 0.5346(4) 0.131(4) Uani 1 1 d . U . . .
H15A H 0.0375 0.4084 0.5466 0.158 Uiso 1 1 calc R U . . .
C16 C 0.0383(6) 0.3108(11) 0.4776(4) 0.148(4) Uani 1 1 d . U . . .
H16A H 0.0300 0.3722 0.4513 0.177 Uiso 1 1 calc R U . . .
C17 C 0.0464(5) 0.1995(11) 0.4615(4) 0.120(3) Uani 1 1 d . U . . .
C18 C 0.0667(6) 0.1185(10) 0.4988(4) 0.135(3) Uani 1 1 d . U . . .
H18A H 0.0818 0.0454 0.4883 0.162 Uiso 1 1 calc R U . . .
C19 C 0.0663(6) 0.1392(9) 0.5566(4) 0.123(3) Uani 1 1 d . U . . .
H19A H 0.0746 0.0772 0.5826 0.148 Uiso 1 1 calc R U . . .
C20 C 0.0396(6) 0.1743(13) 0.3983(4) 0.184(5) Uani 1 1 d . U . . .
H20A H 0.0225 0.2440 0.3763 0.275 Uiso 1 1 calc R U . . .
H20B H 0.0033 0.1119 0.3854 0.275 Uiso 1 1 calc R U . . .
H20C H 0.0885 0.1510 0.3938 0.275 Uiso 1 1 calc R U . . .
N3 N 0.3492(4) 0.6532(5) 0.5355(2) 0.0786(16) Uani 1 1 d . . . . .
C21 C 0.3733(3) 0.7124(6) 0.5089(2) 0.0617(16) Uani 1 1 d . . . . .
N4 N 0.4080(3) 0.7793(6) 0.4817(2) 0.095(2) Uani 1 1 d . . . . .
C22 C 0.3716(3) 0.8423(6) 0.4399(2) 0.0592(15) Uani 1 1 d . . . . .
N5 N 0.3472(3) 0.8996(5) 0.4028(2) 0.0707(15) Uani 1 1 d . . . . .
N6 N 0.2597(4) 0.4067(5) 0.5090(2) 0.0776(16) Uani 1 1 d . . . . .
C23 C 0.2404(5) 0.3511(6) 0.4709(3) 0.085(2) Uani 1 1 d . . . . .
N7 N 0.2090(5) 0.2989(8) 0.4247(3) 0.171(5) Uani 1 1 d . . . . .
C24 C 0.2387(4) 0.2138(6) 0.4029(2) 0.0752(19) Uani 1 1 d . . . . .
N8 N 0.2547(3) 0.1452(5) 0.37927(19) 0.0707(15) Uani 1 1 d . . . . .
O9 O 0.4098(3) 0.4272(5) 0.59853(19) 0.0852(15) Uani 1 1 d D U . . .
H9 H 0.415(4) 0.397(6) 0.6335(19) 0.102 Uiso 1 1 d D U . . .
C25 C 0.4795(7) 0.4388(13) 0.5854(6) 0.201(6) Uani 1 1 d . U . . .
H25A H 0.5129 0.3757 0.6028 0.301 Uiso 1 1 calc R U . . .
H25B H 0.5024 0.5130 0.5995 0.301 Uiso 1 1 calc R U . . .
H25C H 0.4716 0.4358 0.5447 0.301 Uiso 1 1 calc R U . . .
O10 O 0.1930(3) 0.6136(4) 0.56037(17) 0.0789(13) Uani 1 1 d D U . . .
H10 H 0.176(4) 0.617(6) 0.591(2) 0.095 Uiso 1 1 d D U . . .
C26 C 0.1618(7) 0.6974(14) 0.5220(6) 0.225(8) Uani 1 1 d . U . . .
H26A H 0.1118 0.7170 0.5258 0.338 Uiso 1 1 calc R U . . .
H26B H 0.1577 0.6686 0.4842 0.338 Uiso 1 1 calc R U . . .
H26C H 0.1936 0.7664 0.5288 0.338 Uiso 1 1 calc R U . . .
O11 O 0.1931(2) 0.5804(3) 0.80821(16) 0.0583(10) Uani 1 1 d D U . . .
H11 H 0.185(3) 0.602(5) 0.7740(16) 0.070 Uiso 1 1 d D U . . .
C27 C 0.1256(5) 0.5374(9) 0.8152(4) 0.134(4) Uani 1 1 d . U . . .
H27A H 0.0856 0.5936 0.8009 0.201 Uiso 1 1 calc R U . . .
H27B H 0.1306 0.5237 0.8550 0.201 Uiso 1 1 calc R U . . .
H27C H 0.1134 0.4646 0.7946 0.201 Uiso 1 1 calc R U . . .
O12 O 0.4086(3) 0.3910(5) 0.85001(17) 0.0877(16) Uani 1 1 d D . . . .
H12 H 0.430(4) 0.395(6) 0.8207(18) 0.105 Uiso 1 1 d D U . . .
C28A C 0.4637(7) 0.3495(12) 0.8918(5) 0.075(4) Uiso 0.53 1 d D . P A 1
H28A H 0.5018 0.3129 0.8765 0.113 Uiso 0.53 1 calc R U P A 1
H28B H 0.4432 0.2923 0.9129 0.113 Uiso 0.53 1 calc R U P A 1
H28C H 0.4866 0.4128 0.9167 0.113 Uiso 0.53 1 calc R U P A 1
C28B C 0.4370(10) 0.2915(13) 0.8779(7) 0.088(5) Uiso 0.47 1 d D . P A 2
H28D H 0.4882 0.2789 0.8748 0.132 Uiso 0.47 1 calc R U P A 2
H28E H 0.4055 0.2259 0.8615 0.132 Uiso 0.47 1 calc R U P A 2
H28F H 0.4377 0.2989 0.9174 0.132 Uiso 0.47 1 calc R U P A 2
N9 N 0.1241(4) 0.9543(6) 0.7807(3) 0.0935(19) Uani 1 1 d . . . . .
H91 H 0.1595 0.9806 0.7589 0.112 Uiso 1 1 calc R U . . .
C29 C 0.0991(5) 1.0581(7) 0.8049(3) 0.107(3) Uani 1 1 d . . . . .
H29A H 0.1422 1.0950 0.8307 0.161 Uiso 1 1 calc R U . . .
H29B H 0.0623 1.0362 0.8252 0.161 Uiso 1 1 calc R U . . .
H29C H 0.0761 1.1122 0.7749 0.161 Uiso 1 1 calc R U . . .
C30 C 0.0598(5) 0.8972(7) 0.7405(4) 0.106(3) Uani 1 1 d . . . . .
H30A H 0.0777 0.8289 0.7245 0.159 Uiso 1 1 calc R U . . .
H30B H 0.0370 0.9514 0.7104 0.159 Uiso 1 1 calc R U . . .
H30C H 0.0225 0.8738 0.7600 0.159 Uiso 1 1 calc R U . . .
C31 C 0.1649(7) 0.8662(8) 0.8221(5) 0.129(4) Uani 1 1 d . . . . .
H31A H 0.1304 0.8373 0.8435 0.155 Uiso 1 1 calc R U . . .
H31B H 0.1780 0.8001 0.8012 0.155 Uiso 1 1 calc R U . . .
C32 C 0.2331(7) 0.9076(13) 0.8615(5) 0.178(6) Uani 1 1 d . . . . .
H32A H 0.2554 0.8449 0.8871 0.266 Uiso 1 1 calc R U . . .
H32B H 0.2209 0.9724 0.8830 0.266 Uiso 1 1 calc R U . . .
H32C H 0.2688 0.9333 0.8410 0.266 Uiso 1 1 calc R U . . .
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'
S S 0.1246 0.1234 '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'
Br Br -0.2901 2.4595 '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
O3 Mn1 O1 70.74(11) . .
O3 Mn1 N6 95.80(16) . .
O1 Mn1 N6 166.49(17) . .
O3 Mn1 N3 166.28(17) . .
O1 Mn1 N3 95.55(17) . .
N6 Mn1 N3 97.9(2) . .
O3 Mn1 O10 88.40(15) . .
O1 Mn1 O10 88.16(15) . .
N6 Mn1 O10 90.5(2) . .
N3 Mn1 O10 91.5(2) . .
O3 Mn1 O9 90.40(15) . .
O1 Mn1 O9 92.14(16) . .
N6 Mn1 O9 88.9(2) . .
N3 Mn1 O9 89.9(2) . .
O10 Mn1 O9 178.6(2) . .
O1 Mn2 O2 95.91(13) . .
O1 Mn2 O3 83.32(13) . .
O2 Mn2 O3 169.93(14) . .
O1 Mn2 O4 170.35(14) . .
O2 Mn2 O4 83.02(13) . .
O3 Mn2 O4 96.05(13) . .
O1 Mn2 Br1 96.00(11) . .
O2 Mn2 Br1 95.56(11) . .
O3 Mn2 Br1 94.50(10) . .
O4 Mn2 Br1 93.64(10) . .
O1 Mn2 Br2 83.58(11) . .
O2 Mn2 Br2 86.95(11) . .
O3 Mn2 Br2 82.98(10) . .
O4 Mn2 Br2 86.79(10) . .
Br1 Mn2 Br2 177.48(3) . .
Mn1 Mn2 Br2 86.29(2) . .
Mn3 Mn2 Br2 89.77(2) . .
O2 Mn3 N5 94.92(16) . 4_576
O2 Mn3 O4 70.68(11) . .
N5 Mn3 O4 165.59(16) 4_576 .
O2 Mn3 N8 166.65(16) . 4_566
N5 Mn3 N8 98.18(19) 4_576 4_566
O4 Mn3 N8 96.23(16) . 4_566
O2 Mn3 O12 90.88(16) . .
N5 Mn3 O12 90.7(2) 4_576 .
O4 Mn3 O12 89.08(15) . .
N8 Mn3 O12 91.5(2) 4_566 .
O2 Mn3 O11 84.30(13) . .
N5 Mn3 O11 92.93(19) 4_576 .
O4 Mn3 O11 86.32(14) . .
N8 Mn3 O11 92.45(19) 4_566 .
O12 Mn3 O11 174.22(14) . .
C1 O1 Mn2 123.5(3) . .
C1 O1 Mn1 129.3(3) . .
Mn2 O1 Mn1 102.49(13) . .
O1 C1 C3 112.3(4) . .
O1 C1 H1A 109.1 . .
C3 C1 H1A 109.1 . .
O1 C1 H1B 109.1 . .
C3 C1 H1B 109.1 . .
H1A C1 H1B 107.9 . .
C2 O2 Mn2 123.6(3) . .
C2 O2 Mn3 128.9(3) . .
Mn2 O2 Mn3 103.26(14) . .
O2 C2 C3 111.5(4) . .
O2 C2 H2A 109.3 . .
C3 C2 H2A 109.3 . .
O2 C2 H2B 109.3 . .
C3 C2 H2B 109.3 . .
H2A C2 H2B 108.0 . .
N1 C3 C2 110.7(4) . .
N1 C3 C1 112.4(5) . .
C2 C3 C1 112.8(4) . .
N1 C3 H3A 106.8 . .
C2 C3 H3A 106.8 . .
C1 C3 H3A 106.8 . .
C3 N1 S1 120.5(4) . .
C3 N1 H1 120(5) . .
S1 N1 H1 109(5) . .
O5 S1 O6 118.0(3) . .
O5 S1 N1 105.4(3) . .
O6 S1 N1 109.0(3) . .
O5 S1 C4 108.4(3) . .
O6 S1 C4 107.4(3) . .
N1 S1 C4 108.4(3) . .
C5 C4 C9 120.1(6) . .
C5 C4 S1 120.2(6) . .
C9 C4 S1 119.7(5) . .
C4 C5 C6 120.4(7) . .
C4 C5 H5A 119.8 . .
C6 C5 H5A 119.8 . .
C7 C6 C5 120.2(7) . .
C7 C6 H6A 119.9 . .
C5 C6 H6A 119.9 . .
C8 C7 C6 117.4(6) . .
C8 C7 C10 121.9(6) . .
C6 C7 C10 120.7(6) . .
C7 C8 C9 121.9(6) . .
C7 C8 H8A 119.0 . .
C9 C8 H8A 119.0 . .
C4 C9 C8 119.9(6) . .
C4 C9 H9A 120.0 . .
C8 C9 H9A 120.0 . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C11 O3 Mn2 123.1(3) . .
C11 O3 Mn1 129.0(3) . .
Mn2 O3 Mn1 102.46(13) . .
O3 C11 C13 112.7(4) . .
O3 C11 H11A 109.0 . .
C13 C11 H11A 109.0 . .
O3 C11 H11B 109.0 . .
C13 C11 H11B 109.0 . .
H11A C11 H11B 107.8 . .
C12 O4 Mn2 122.6(3) . .
C12 O4 Mn3 129.6(3) . .
Mn2 O4 Mn3 102.48(13) . .
O4 C12 C13 111.7(4) . .
O4 C12 H12A 109.3 . .
C13 C12 H12A 109.3 . .
O4 C12 H12B 109.3 . .
C13 C12 H12B 109.3 . .
H12A C12 H12B 107.9 . .
N2 C13 C11 112.7(4) . .
N2 C13 C12 108.4(4) . .
C11 C13 C12 112.9(4) . .
N2 C13 H13A 107.5 . .
C11 C13 H13A 107.5 . .
C12 C13 H13A 107.5 . .
C13 N2 S2 121.2(4) . .
C13 N2 H2 118(4) . .
S2 N2 H2 116(4) . .
O7 S2 O8 119.9(4) . .
O7 S2 N2 108.8(3) . .
O8 S2 N2 106.7(3) . .
O7 S2 C14 105.5(4) . .
O8 S2 C14 107.7(4) . .
N2 S2 C14 107.7(3) . .
C19 C14 C15 118.9(8) . .
C19 C14 S2 121.5(8) . .
C15 C14 S2 119.6(6) . .
C14 C15 C16 121.7(10) . .
C14 C15 H15A 119.2 . .
C16 C15 H15A 119.2 . .
C17 C16 C15 118.0(11) . .
C17 C16 H16A 121.0 . .
C15 C16 H16A 121.0 . .
C18 C17 C16 120.3(9) . .
C18 C17 C20 120.6(11) . .
C16 C17 C20 118.8(11) . .
C17 C18 C19 120.4(10) . .
C17 C18 H18A 119.8 . .
C19 C18 H18A 119.8 . .
C14 C19 C18 119.6(10) . .
C14 C19 H19A 120.2 . .
C18 C19 H19A 120.2 . .
C17 C20 H20A 109.5 . .
C17 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C17 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C21 N3 Mn1 172.9(6) . .
N3 C21 N4 174.0(7) . .
C22 N4 C21 121.5(6) . .
N5 C22 N4 172.6(7) . .
C22 N5 Mn3 177.7(6) . 4_575
C23 N6 Mn1 175.4(6) . .
N6 C23 N7 170.5(9) . .
C23 N7 C24 125.3(8) . .
N8 C24 N7 170.2(8) . .
C24 N8 Mn3 172.7(6) . 4_565
C25 O9 Mn1 136.4(6) . .
C25 O9 H9 112(5) . .
Mn1 O9 H9 105(5) . .
O9 C25 H25A 109.5 . .
O9 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
O9 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C26 O10 Mn1 132.5(6) . .
C26 O10 H10 112(5) . .
Mn1 O10 H10 110(5) . .
O10 C26 H26A 109.5 . .
O10 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
O10 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C27 O11 Mn3 123.5(5) . .
C27 O11 H11 107(4) . .
Mn3 O11 H11 109(4) . .
O11 C27 H27A 109.5 . .
O11 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
O11 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C28A O12 Mn3 141.7(6) . .
C28B O12 Mn3 135.2(8) . .
C28A O12 H12 103(5) . .
C28B O12 H12 105(5) . .
Mn3 O12 H12 113(5) . .
O12 C28A H28A 109.5 . .
O12 C28A H28B 109.5 . .
H28A C28A H28B 109.5 . .
O12 C28A H28C 109.5 . .
H28A C28A H28C 109.5 . .
H28B C28A H28C 109.5 . .
O12 C28B H28D 109.5 . .
O12 C28B H28E 109.5 . .
H28D C28B H28E 109.5 . .
O12 C28B H28F 109.5 . .
H28D C28B H28F 109.5 . .
H28E C28B H28F 109.5 . .
C29 N9 C30 110.8(7) . .
C29 N9 C31 115.6(7) . .
C30 N9 C31 109.0(7) . .
C29 N9 H91 107.0 . .
C30 N9 H91 107.0 . .
C31 N9 H91 107.0 . .
N9 C29 H29A 109.5 . .
N9 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
N9 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
N9 C30 H30A 109.5 . .
N9 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
N9 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C32 C31 N9 115.2(9) . .
C32 C31 H31A 108.5 . .
N9 C31 H31A 108.5 . .
C32 C31 H31B 108.5 . .
N9 C31 H31B 108.5 . .
H31A C31 H31B 107.5 . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O3 2.163(3) .
Mn1 O1 2.166(3) .
Mn1 N6 2.173(5) .
Mn1 N3 2.175(5) .
Mn1 O10 2.216(5) .
Mn1 O9 2.218(5) .
Mn1 Mn2 3.1626(9) .
Mn2 O1 1.883(3) .
Mn2 O2 1.884(3) .
Mn2 O3 1.887(3) .
Mn2 O4 1.890(3) .
Mn2 Br1 2.7370(9) .
Mn2 Mn3 3.1708(9) .
Mn2 Br2 3.3621(9) .
Mn3 O2 2.154(3) .
Mn3 N5 2.166(5) 4_576
Mn3 O4 2.170(3) .
Mn3 N8 2.188(5) 4_566
Mn3 O12 2.204(4) .
Mn3 O11 2.229(4) .
O1 C1 1.409(6) .
C1 C3 1.518(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
O2 C2 1.423(6) .
C2 C3 1.514(7) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 N1 1.420(7) .
C3 H3A 1.0000 .
N1 S1 1.610(5) .
N1 H1 0.84(3) .
S1 O5 1.421(6) .
S1 O6 1.430(5) .
S1 C4 1.749(6) .
C4 C5 1.337(9) .
C4 C9 1.352(9) .
C5 C6 1.396(10) .
C5 H5A 0.9500 .
C6 C7 1.384(9) .
C6 H6A 0.9500 .
C7 C8 1.357(9) .
C7 C10 1.514(8) .
C8 C9 1.377(8) .
C8 H8A 0.9500 .
C9 H9A 0.9500 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
O3 C11 1.412(5) .
C11 C13 1.511(6) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
O4 C12 1.408(5) .
C12 C13 1.525(7) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 N2 1.444(7) .
C13 H13A 1.0000 .
N2 S2 1.605(5) .
N2 H2 0.84(3) .
S2 O7 1.391(6) .
S2 O8 1.428(6) .
S2 C14 1.747(7) .
C14 C19 1.323(10) .
C14 C15 1.357(12) .
C15 C16 1.416(11) .
C15 H15A 0.9500 .
C16 C17 1.368(14) .
C16 H16A 0.9500 .
C17 C18 1.302(14) .
C17 C20 1.567(12) .
C18 C19 1.453(13) .
C18 H18A 0.9500 .
C19 H19A 0.9500 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
N3 C21 1.121(7) .
C21 N4 1.303(8) .
N4 C22 1.301(8) .
C22 N5 1.128(7) .
N5 Mn3 2.166(5) 4_575
N6 C23 1.122(8) .
C23 N7 1.291(9) .
N7 C24 1.311(9) .
C24 N8 1.074(7) .
N8 Mn3 2.188(5) 4_565
O9 C25 1.417(11) .
O9 H9 0.92(4) .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
O10 C26 1.375(11) .
O10 H10 0.90(4) .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
O11 C27 1.396(8) .
O11 H11 0.86(3) .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
O12 C28A 1.338(11) .
O12 C28B 1.375(13) .
O12 H12 0.92(3) .
C28A H28A 0.9800 .
C28A H28B 0.9800 .
C28A H28C 0.9800 .
C28B H28D 0.9800 .
C28B H28E 0.9800 .
C28B H28F 0.9800 .
N9 C29 1.471(9) .
N9 C30 1.491(10) .
N9 C31 1.501(10) .
N9 H91 1.0000 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 C32 1.459(15) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 Br2 0.84(3) 2.76(5) 3.507(5) 148(5) .
N2 H2 Br2 0.84(3) 2.66(4) 3.500(5) 177(5) .
O9 H9 Br1 0.92(4) 2.30(4) 3.185(4) 161(6) .
O10 H10 Br2 0.90(4) 2.34(4) 3.235(4) 175(7) .
O11 H11 Br2 0.86(3) 2.42(4) 3.262(4) 168(6) .
O12 H12 Br1 0.92(3) 2.33(3) 3.199(4) 159(6) .
N9 H91 O5 1.00 1.89 2.835(7) 155.6 .
C3 H3A Br1 1.00 2.79 3.659(6) 145.9 2_656
C13 H13A O5 1.00 2.58 3.490(7) 151.4 1_545
C29 H29A N7 0.98 2.64 3.538(12) 153.1 4_576
C29 H29B O8 0.98 2.57 3.408(10) 143.0 2_556
C30 H30C O8 0.98 2.60 3.426(9) 141.9 2_556
C31 H31A O8 0.99 2.54 3.398(12) 144.4 2_556
C31 H31B O11 0.99 2.56 3.382(10) 140.4 .
