# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Li Baolong'
_publ_contact_author_email       LIBAOLONG@SUDA.EDU.CN

_publ_section_title              
;
Solvent-controlled assembly of supramolecular isomers:
2D (4,4) network, 1D ribbons of ring, and both 2D (4,4) networks and
1D ribbons of rings polycatenated in a 3D array
;
loop_
_publ_author_name
'Li Baolong'
'Xun-Gao Liu'
'Yong Zhang'
'Xia Zhu'

data_[Mn(btb)2(NCS)2](CH2Cl2)(1)
_database_code_depnum_ccdc_archive 'CCDC 714832'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H26 Cl2 Mn N14 S2'
_chemical_formula_weight         640.50
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'
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'
S S 0.1246 0.1234 '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'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   8.4645(18)
_cell_length_b                   9.117(2)
_cell_length_c                   11.632(2)
_cell_angle_alpha                110.885(6)
_cell_angle_beta                 90.108(3)
_cell_angle_gamma                104.698(5)
_cell_volume                     807.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    3175
_cell_measurement_theta_min      3.0088
_cell_measurement_theta_max      25.3491
_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             329
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7824
_exptl_absorpt_correction_T_max  0.8726
_exptl_absorpt_process_details   Empirical
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7973
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         25.35
_reflns_number_total             2905
_reflns_number_gt                2592
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and Rfactors
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1161P)²+2.2976P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2905
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.2080
_refine_ls_wR_factor_gt          0.2019
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
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 0.0000 0.0000 0.0000 0.0209(3) Uani 1 2 d S . .
S1 S 0.1648(3) 0.58689(17) 0.25003(17) 0.0712(6) Uani 1 1 d . . .
N1 N 0.4186(4) -0.1643(4) 0.0792(3) 0.0261(7) Uani 1 1 d . . .
N2 N 0.4754(4) -0.0019(4) 0.1518(3) 0.0318(8) Uani 1 1 d . . .
N3 N 0.2334(4) -0.0532(4) 0.0453(3) 0.0260(7) Uani 1 1 d . . .
N4 N -0.1889(4) 0.0188(4) 0.3555(3) 0.0310(8) Uani 1 1 d . . .
N5 N -0.1350(5) -0.1171(5) 0.3320(4) 0.0392(9) Uani 1 1 d . . .
N6 N -0.0772(4) -0.0143(4) 0.1833(3) 0.0261(7) Uani 1 1 d . . .
N7 N 0.1104(5) 0.2624(4) 0.0926(4) 0.0333(8) Uani 1 1 d . . .
C1 C 0.5146(5) -0.2752(5) 0.0855(4) 0.0323(10) Uani 1 1 d . . .
H1A H 0.5134 -0.2809 0.1689 0.039 Uiso 1 1 calc R . .
H1B H 0.6300 -0.2301 0.0735 0.039 Uiso 1 1 calc R . .
C2 C 0.4503(5) -0.4452(5) -0.0099(4) 0.0289(9) Uani 1 1 d . . .
H2A H 0.4600 -0.4424 -0.0940 0.035 Uiso 1 1 calc R . .
H2B H 0.3329 -0.4892 -0.0022 0.035 Uiso 1 1 calc R . .
C3 C 0.3594(5) 0.0571(5) 0.1279(4) 0.0295(9) Uani 1 1 d . . .
H3A H 0.3631 0.1692 0.1657 0.035 Uiso 1 1 calc R . .
C4 C 0.2758(5) -0.1916(5) 0.0175(4) 0.0285(9) Uani 1 1 d . . .
H4A H 0.2128 -0.2951 -0.0384 0.034 Uiso 1 1 calc R . .
C5 C -0.2787(6) 0.0759(6) 0.4630(4) 0.0387(11) Uani 1 1 d . . .
H5A H -0.2798 0.1897 0.4786 0.046 Uiso 1 1 calc R . .
H5B H -0.2212 0.0751 0.5369 0.046 Uiso 1 1 calc R . .
C6 C -0.4544(5) -0.0303(6) 0.4435(4) 0.0350(10) Uani 1 1 d . . .
H6A H -0.4538 -0.1443 0.4277 0.042 Uiso 1 1 calc R . .
H6B H -0.5125 -0.0289 0.3701 0.042 Uiso 1 1 calc R . .
C7 C -0.0698(6) -0.1307(6) 0.2274(4) 0.0348(10) Uani 1 1 d . . .
H7A H -0.0212 -0.2161 0.1861 0.042 Uiso 1 1 calc R . .
C8 C -0.1545(5) 0.0769(5) 0.2666(4) 0.0273(9) Uani 1 1 d . . .
H8A H -0.1812 0.1703 0.2629 0.033 Uiso 1 1 calc R . .
C9 C 0.1314(5) 0.3970(5) 0.1579(4) 0.0300(9) Uani 1 1 d . . .
Cl1 Cl 0.2557(4) 0.2660(4) 0.4176(3) 0.0641(8) Uani 0.50 1 d P . .
Cl2 Cl 0.3272(5) 0.5581(5) 0.6432(4) 0.0863(11) Uani 0.50 1 d P . .
C10 C 0.1881(15) 0.3871(15) 0.5210(15) 0.071(4) Uani 0.50 1 d P . .
H10B H 0.1123 0.3231 0.5614 0.085 Uiso 0.50 1 calc PR . .
H10A H 0.1209 0.4331 0.4806 0.085 Uiso 0.50 1 calc PR . .
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate
(isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N7 2.187(4) 2 ?
Mn1 N7 2.187(4) . ?
Mn1 N3 2.254(3) 2 ?
Mn1 N3 2.254(3) . ?
Mn1 N6 2.269(3) 2 ?
Mn1 N6 2.269(3) . ?
S1 C9 1.628(4) . ?
N1 C4 1.325(5) . ?
N1 N2 1.372(5) . ?
N1 C1 1.468(5) . ?
N2 C3 1.306(6) . ?
N3 C4 1.329(5) . ?
N3 C3 1.354(5) . ?
N4 C8 1.322(5) . ?
N4 N5 1.365(5) . ?
N4 C5 1.467(5) . ?
N5 C7 1.315(6) . ?
N6 C8 1.328(5) . ?
N6 C7 1.347(6) . ?
N7 C9 1.158(6) . ?
C1 C2 1.508(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C2 1.534(8) 2_645 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9500 . ?
C4 H4A 0.9500 . ?
C5 C6 1.520(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C6 1.526(8) 2_456 ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
Cl1 C10 1.539(16) . ?
Cl2 C10 1.822(14) . ?
C10 H10B 0.9900 . ?
C10 H10A 0.9900 . ?
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
N7 Mn1 N7 180.00(12) 2 . ?
N7 Mn1 N3 91.13(13) 2 2 ?
N7 Mn1 N3 88.87(13) . 2 ?
N7 Mn1 N3 88.87(13) 2 . ?
N7 Mn1 N3 91.13(13) . . ?
N3 Mn1 N3 180.00(17) 2 . ?
N7 Mn1 N6 89.65(13) 2 2 ?
N7 Mn1 N6 90.35(13) . 2 ?
N3 Mn1 N6 87.01(12) 2 2 ?
N3 Mn1 N6 92.99(12) . 2 ?
N7 Mn1 N6 90.35(13) 2 . ?
N7 Mn1 N6 89.65(13) . . ?
N3 Mn1 N6 92.99(12) 2 . ?
N3 Mn1 N6 87.01(12) . . ?
N6 Mn1 N6 180.0(3) 2 . ?
C4 N1 N2 109.8(3) . . ?
C4 N1 C1 131.6(4) . . ?
N2 N1 C1 118.5(3) . . ?
C3 N2 N1 102.2(3) . . ?
C4 N3 C3 102.8(3) . . ?
C4 N3 Mn1 132.1(3) . . ?
C3 N3 Mn1 124.4(3) . . ?
C8 N4 N5 109.9(3) . . ?
C8 N4 C5 129.0(4) . . ?
N5 N4 C5 121.0(4) . . ?
C7 N5 N4 102.2(4) . . ?
C8 N6 C7 102.9(3) . . ?
C8 N6 Mn1 129.6(3) . . ?
C7 N6 Mn1 127.2(3) . . ?
C9 N7 Mn1 161.6(3) . . ?
N1 C1 C2 113.0(3) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 C2 109.2(4) . 2_645 ?
C1 C2 H2A 109.8 . . ?
C2 C2 H2A 109.8 2_645 . ?
C1 C2 H2B 109.8 . . ?
C2 C2 H2B 109.8 2_645 . ?
H2A C2 H2B 108.3 . . ?
N2 C3 N3 115.1(4) . . ?
N2 C3 H3A 122.4 . . ?
N3 C3 H3A 122.4 . . ?
N1 C4 N3 110.0(4) . . ?
N1 C4 H4A 125.0 . . ?
N3 C4 H4A 125.0 . . ?
N4 C5 C6 111.9(4) . . ?
N4 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
N4 C5 H5B 109.2 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C5 C6 C6 111.1(5) . 2_456 ?
C5 C6 H6A 109.4 . . ?
C6 C6 H6A 109.4 2_456 . ?
C5 C6 H6B 109.4 . . ?
C6 C6 H6B 109.4 2_456 . ?
H6A C6 H6B 108.0 . . ?
N5 C7 N6 114.8(4) . . ?
N5 C7 H7A 122.6 . . ?
N6 C7 H7A 122.6 . . ?
N4 C8 N6 110.1(4) . . ?
N4 C8 H8A 124.9 . . ?
N6 C8 H8A 124.9 . . ?
N7 C9 S1 178.9(4) . . ?
Cl1 C10 Cl2 120.5(8) . . ?
Cl1 C10 H10B 107.2 . . ?
Cl2 C10 H10B 107.2 . . ?
Cl1 C10 H10A 107.2 . . ?
Cl2 C10 H10A 107.2 . . ?
H10B C10 H10A 106.8 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 N2 C3 0.2(4) . . . . ?
C1 N1 N2 C3 -177.1(4) . . . . ?
N7 Mn1 N3 C4 2.7(4) 2 . . . ?
N7 Mn1 N3 C4 -177.3(4) . . . . ?
N6 Mn1 N3 C4 -86.9(4) 2 . . . ?
N6 Mn1 N3 C4 93.1(4) . . . . ?
N7 Mn1 N3 C3 -166.5(3) 2 . . . ?
N7 Mn1 N3 C3 13.5(3) . . . . ?
N6 Mn1 N3 C3 103.9(3) 2 . . . ?
N6 Mn1 N3 C3 -76.1(3) . . . . ?
C8 N4 N5 C7 0.1(5) . . . . ?
C5 N4 N5 C7 177.0(4) . . . . ?
N7 Mn1 N6 C8 -130.9(4) 2 . . . ?
N7 Mn1 N6 C8 49.1(4) . . . . ?
N3 Mn1 N6 C8 -39.7(4) 2 . . . ?
N3 Mn1 N6 C8 140.3(4) . . . . ?
N7 Mn1 N6 C7 41.6(4) 2 . . . ?
N7 Mn1 N6 C7 -138.4(4) . . . . ?
N3 Mn1 N6 C7 132.7(4) 2 . . . ?
N3 Mn1 N6 C7 -47.3(4) . . . . ?
N3 Mn1 N7 C9 53.5(11) 2 . . . ?
N3 Mn1 N7 C9 -126.5(11) . . . . ?
N6 Mn1 N7 C9 140.5(11) 2 . . . ?
N6 Mn1 N7 C9 -39.5(11) . . . . ?
C4 N1 C1 C2 10.5(7) . . . . ?
N2 N1 C1 C2 -172.8(4) . . . . ?
N1 C1 C2 C2 -175.8(4) . . . 2_645 ?
N1 N2 C3 N3 -0.5(5) . . . . ?
C4 N3 C3 N2 0.6(5) . . . . ?
Mn1 N3 C3 N2 172.4(3) . . . . ?
N2 N1 C4 N3 0.2(5) . . . . ?
C1 N1 C4 N3 177.1(4) . . . . ?
C3 N3 C4 N1 -0.5(5) . . . . ?
Mn1 N3 C4 N1 -171.3(3) . . . . ?
C8 N4 C5 C6 101.3(5) . . . . ?
N5 N4 C5 C6 -74.9(5) . . . . ?
N4 C5 C6 C6 179.7(5) . . . 2_456 ?
N4 N5 C7 N6 0.3(5) . . . . ?
C8 N6 C7 N5 -0.7(5) . . . . ?
Mn1 N6 C7 N5 -174.7(3) . . . . ?
N5 N4 C8 N6 -0.6(5) . . . . ?
C5 N4 C8 N6 -177.1(4) . . . . ?
C7 N6 C8 N4 0.7(5) . . . . ?
Mn1 N6 C8 N4 174.5(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.854
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.118
###======

data_[Mn(btb)2(NCS)2](CH3NO2)2(2)
_database_code_depnum_ccdc_archive 'CCDC 714833'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H30 Mn N16 O4 S2'
_chemical_formula_weight         677.66
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'
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'
S S 0.1246 0.1234 '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'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   8.6873(10)
_cell_length_b                   8.9324(11)
_cell_length_c                   10.5653(15)
_cell_angle_alpha                82.685(8)
_cell_angle_beta                 84.302(9)
_cell_angle_gamma                70.617(6)
_cell_volume                     765.66(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2717
_cell_measurement_theta_min      3.0677
_cell_measurement_theta_max      25.3491
_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             351
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8349
_exptl_absorpt_correction_T_max  0.9402
_exptl_absorpt_process_details   Empirical
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7599
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.34
_reflns_number_total             2791
_reflns_number_gt                2387
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and Rfactors
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0446P)²+0.3811P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2791
_refine_ls_number_parameters     197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
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 0.0000 0.5000 0.0000 0.01930(15) Uani 1 2 d S . .
S1 S 0.55201(8) 0.18429(10) 0.12975(6) 0.0421(2) Uani 1 1 d . . .
O1 O 0.0794(3) 0.2804(3) 0.5267(3) 0.0856(9) Uani 1 1 d . . .
O2 O 0.3349(3) 0.1845(2) 0.5505(2) 0.0549(6) Uani 1 1 d . . .
N1 N 0.1907(2) 0.8265(2) 0.16464(17) 0.0230(4) Uani 1 1 d . . .
N2 N 0.0328(2) 0.9220(2) 0.16701(19) 0.0299(5) Uani 1 1 d . . .
N3 N 0.0578(2) 0.6884(2) 0.09464(17) 0.0238(4) Uani 1 1 d . . .
N4 N 0.2313(2) 0.6982(2) 0.66069(17) 0.0226(4) Uani 1 1 d . . .
N5 N 0.3182(3) 0.5418(2) 0.6500(2) 0.0354(5) Uani 1 1 d . . .
N6 N 0.1346(2) 0.5668(2) 0.81823(17) 0.0234(4) Uani 1 1 d . . .
N7 N 0.2328(2) 0.3204(2) 0.05316(19) 0.0302(5) Uani 1 1 d . . .
N8 N 0.2183(3) 0.2758(3) 0.4969(2) 0.0377(5) Uani 1 1 d . . .
C1 C 0.3198(3) 0.8815(3) 0.2015(2) 0.0286(5) Uani 1 1 d . . .
H1A H 0.3249 0.9758 0.1430 0.034 Uiso 1 1 calc R . .
H1B H 0.4265 0.7963 0.1925 0.034 Uiso 1 1 calc R . .
C2 C 0.2903(3) 0.9252(3) 0.3387(2) 0.0254(5) Uani 1 1 d . . .
H2A H 0.3800 0.9615 0.3594 0.030 Uiso 1 1 calc R . .
H2B H 0.1868 1.0149 0.3463 0.030 Uiso 1 1 calc R . .
C3 C 0.2810(3) 0.7855(3) 0.4343(2) 0.0255(5) Uani 1 1 d . . .
H3A H 0.1868 0.7538 0.4170 0.031 Uiso 1 1 calc R . .
H3B H 0.3815 0.6936 0.4228 0.031 Uiso 1 1 calc R . .
C4 C 0.2624(3) 0.8257(3) 0.5714(2) 0.0261(5) Uani 1 1 d . . .
H4A H 0.3635 0.8426 0.5928 0.031 Uiso 1 1 calc R . .
H4B H 0.1708 0.9262 0.5804 0.031 Uiso 1 1 calc R . .
C5 C -0.0418(3) 0.8343(3) 0.1241(2) 0.0281(5) Uani 1 1 d . . .
H5A H -0.1563 0.8700 0.1144 0.034 Uiso 1 1 calc R . .
C6 C 0.2039(3) 0.6887(3) 0.1217(2) 0.0239(5) Uani 1 1 d . . .
H6A H 0.3031 0.6032 0.1119 0.029 Uiso 1 1 calc R . .
C7 C 0.2543(3) 0.4694(3) 0.7460(2) 0.0329(6) Uani 1 1 d . . .
H7A H 0.2894 0.3566 0.7636 0.040 Uiso 1 1 calc R . .
C8 C 0.1248(3) 0.7103(3) 0.7607(2) 0.0226(5) Uani 1 1 d . . .
H8A H 0.0518 0.8079 0.7875 0.027 Uiso 1 1 calc R . .
C9 C 0.3661(3) 0.2637(3) 0.0836(2) 0.0231(5) Uani 1 1 d . . .
C10 C 0.2468(4) 0.3860(4) 0.3892(3) 0.0501(8) Uani 1 1 d . . .
H10A H 0.1421 0.4641 0.3648 0.075 Uiso 1 1 calc R . .
H10B H 0.3000 0.3260 0.3166 0.075 Uiso 1 1 calc R . .
H10C H 0.3174 0.4415 0.4143 0.075 Uiso 1 1 calc R . .
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate
(isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N7 2.196(2) 2_565 ?
Mn1 N7 2.196(2) . ?
Mn1 N6 2.2667(18) 1_554 ?
Mn1 N6 2.2667(18) 2_566 ?
Mn1 N3 2.2740(17) . ?
Mn1 N3 2.2740(17) 2_565 ?
S1 C9 1.630(2) . ?
O1 N8 1.204(3) . ?
O2 N8 1.208(3) . ?
N1 C6 1.331(3) . ?
N1 N2 1.354(3) . ?
N1 C1 1.467(3) . ?
N2 C5 1.314(3) . ?
N3 C6 1.330(3) . ?
N3 C5 1.358(3) . ?
N4 C8 1.324(3) . ?
N4 N5 1.363(3) . ?
N4 C4 1.463(3) . ?
N5 C7 1.310(3) . ?
N6 C8 1.326(3) . ?
N6 C7 1.353(3) . ?
N6 Mn1 2.2667(18) 1_556 ?
N7 C9 1.159(3) . ?
N8 C10 1.465(4) . ?
C1 C2 1.524(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.521(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.517(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
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
N7 Mn1 N7 180.00(15) 2_565 . ?
N7 Mn1 N6 92.56(7) 2_565 1_554 ?
N7 Mn1 N6 87.44(7) . 1_554 ?
N7 Mn1 N6 87.44(7) 2_565 2_566 ?
N7 Mn1 N6 92.56(7) . 2_566 ?
N6 Mn1 N6 180.0 1_554 2_566 ?
N7 Mn1 N3 88.68(7) 2_565 . ?
N7 Mn1 N3 91.32(7) . . ?
N6 Mn1 N3 88.79(6) 1_554 . ?
N6 Mn1 N3 91.21(6) 2_566 . ?
N7 Mn1 N3 91.32(7) 2_565 2_565 ?
N7 Mn1 N3 88.68(7) . 2_565 ?
N6 Mn1 N3 91.21(6) 1_554 2_565 ?
N6 Mn1 N3 88.79(6) 2_566 2_565 ?
N3 Mn1 N3 180.00(8) . 2_565 ?
C6 N1 N2 110.05(18) . . ?
C6 N1 C1 128.9(2) . . ?
N2 N1 C1 120.98(18) . . ?
C5 N2 N1 102.67(18) . . ?
C6 N3 C5 102.60(18) . . ?
C6 N3 Mn1 127.48(15) . . ?
C5 N3 Mn1 129.54(15) . . ?
C8 N4 N5 109.86(18) . . ?
C8 N4 C4 128.62(19) . . ?
N5 N4 C4 121.51(18) . . ?
C7 N5 N4 102.17(19) . . ?
C8 N6 C7 102.46(18) . . ?
C8 N6 Mn1 129.17(15) . 1_556 ?
C7 N6 Mn1 128.23(15) . 1_556 ?
C9 N7 Mn1 160.93(19) . . ?
O1 N8 O2 123.5(3) . . ?
O1 N8 C10 118.1(3) . . ?
O2 N8 C10 118.4(2) . . ?
N1 C1 C2 111.91(18) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C3 C2 C1 112.18(19) . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C2 112.26(18) . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N4 C4 C3 111.37(18) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 N3 114.7(2) . . ?
N2 C5 H5A 122.7 . . ?
N3 C5 H5A 122.7 . . ?
N3 C6 N1 110.0(2) . . ?
N3 C6 H6A 125.0 . . ?
N1 C6 H6A 125.0 . . ?
N5 C7 N6 115.2(2) . . ?
N5 C7 H7A 122.4 . . ?
N6 C7 H7A 122.4 . . ?
N4 C8 N6 110.3(2) . . ?
N4 C8 H8A 124.8 . . ?
N6 C8 H8A 124.8 . . ?
N7 C9 S1 178.7(2) . . ?
N8 C10 H10A 109.5 . . ?
N8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 N2 C5 -0.1(2) . . . . ?
C1 N1 N2 C5 177.77(19) . . . . ?
N7 Mn1 N3 C6 -158.83(19) 2_565 . . . ?
N7 Mn1 N3 C6 21.17(19) . . . . ?
N6 Mn1 N3 C6 -66.24(19) 1_554 . . . ?
N6 Mn1 N3 C6 113.76(19) 2_566 . . . ?
N7 Mn1 N3 C5 12.9(2) 2_565 . . . ?
N7 Mn1 N3 C5 -167.1(2) . . . . ?
N6 Mn1 N3 C5 105.4(2) 1_554 . . . ?
N6 Mn1 N3 C5 -74.6(2) 2_566 . . . ?
C8 N4 N5 C7 0.9(3) . . . . ?
C4 N4 N5 C7 179.7(2) . . . . ?
N6 Mn1 N7 C9 68.1(6) 1_554 . . . ?
N6 Mn1 N7 C9 -111.9(6) 2_566 . . . ?
N3 Mn1 N7 C9 -20.7(6) . . . . ?
N3 Mn1 N7 C9 159.3(6) 2_565 . . . ?
C6 N1 C1 C2 -122.9(2) . . . . ?
N2 N1 C1 C2 59.7(3) . . . . ?
N1 C1 C2 C3 58.8(3) . . . . ?
C1 C2 C3 C4 176.3(2) . . . . ?
C8 N4 C4 C3 -136.8(2) . . . . ?
N5 N4 C4 C3 44.6(3) . . . . ?
C2 C3 C4 N4 172.22(18) . . . . ?
N1 N2 C5 N3 0.2(3) . . . . ?
C6 N3 C5 N2 -0.2(3) . . . . ?
Mn1 N3 C5 N2 -173.41(15) . . . . ?
C5 N3 C6 N1 0.1(2) . . . . ?
Mn1 N3 C6 N1 173.52(14) . . . . ?
N2 N1 C6 N3 0.0(3) . . . . ?
C1 N1 C6 N3 -177.65(19) . . . . ?
N4 N5 C7 N6 -0.7(3) . . . . ?
C8 N6 C7 N5 0.3(3) . . . . ?
Mn1 N6 C7 N5 -175.62(17) 1_556 . . . ?
N5 N4 C8 N6 -0.7(3) . . . . ?
C4 N4 C8 N6 -179.5(2) . . . . ?
C7 N6 C8 N4 0.3(2) . . . . ?
Mn1 N6 C8 N4 176.15(13) 1_556 . . . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.053
###======

data_[2D-Mn(btb)2(NCS)2][1D-Mn(btb)2(NCS)2](3)
_database_code_depnum_ccdc_archive 'CCDC 714834'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H48 Mn2 N28 S4'
_chemical_formula_weight         1111.14
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   9.0938(17)
_cell_length_b                   10.587(2)
_cell_length_c                   13.567(3)
_cell_angle_alpha                103.854(4)
_cell_angle_beta                 100.129(5)
_cell_angle_gamma                99.920(4)
_cell_volume                     1216.7(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    4935
_cell_measurement_theta_min      3.1052
_cell_measurement_theta_max      25.3491
_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             574
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7785
_exptl_absorpt_correction_T_max  0.8827
_exptl_absorpt_process_details   Empirical
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12168
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         25.35
_reflns_number_total             4440
_reflns_number_gt                3951
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and Rfactors
based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0325P)²+0.5106P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4440
_refine_ls_number_parameters     319
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0722
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
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 0.0000 1.0000 0.5000 0.01793(10) Uani 1 2 d S . .
Mn2 Mn 1.0000 0.5000 1.0000 0.01897(10) Uani 1 2 d S . .
S1 S -0.41579(6) 0.62363(5) 0.26838(4) 0.03142(13) Uani 1 1 d . . .
S2 S 1.10509(6) 0.60221(5) 0.67582(4) 0.03300(14) Uani 1 1 d . . .
N1 N 0.29709(16) 0.70601(15) 0.47147(12) 0.0213(3) Uani 1 1 d . . .
N2 N 0.40759(17) 0.81955(15) 0.49354(13) 0.0255(4) Uani 1 1 d . . .
N3 N 0.17525(17) 0.86769(15) 0.49169(12) 0.0214(3) Uani 1 1 d . . .
N4 N 0.01580(17) 0.91486(15) 0.80117(12) 0.0235(3) Uani 1 1 d . . .
N5 N -0.12856(18) 0.83964(17) 0.75668(13) 0.0291(4) Uani 1 1 d . . .
N6 N -0.03938(17) 0.94855(15) 0.64791(12) 0.0225(3) Uani 1 1 d . . .
N7 N -0.18203(18) 0.82814(16) 0.40680(14) 0.0303(4) Uani 1 1 d . . .
N8 N 0.62702(17) 0.68085(15) 0.89527(12) 0.0222(3) Uani 1 1 d . . .
N9 N 0.6036(2) 0.69440(18) 0.99303(13) 0.0336(4) Uani 1 1 d . . .
N10 N 0.79992(17) 0.59530(15) 0.97152(12) 0.0220(3) Uani 1 1 d . . .
N11 N 0.63776(17) 1.15259(15) 0.81987(12) 0.0233(3) Uani 1 1 d . . .
N12 N 0.73206(19) 1.13366(16) 0.75265(13) 0.0301(4) Uani 1 1 d . . .
N13 N 0.84419(17) 1.30945(15) 0.89245(12) 0.0230(3) Uani 1 1 d . . .
N14 N 1.07287(19) 0.54225(17) 0.86171(14) 0.0314(4) Uani 1 1 d . . .
C1 C 0.3285(2) 0.91325(19) 0.50515(15) 0.0245(4) Uani 1 1 d . . .
H1A H 0.3751 1.0055 0.5216 0.029 Uiso 1 1 calc R . .
C2 C 0.1605(2) 0.73621(18) 0.47012(14) 0.0219(4) Uani 1 1 d . . .
H2A H 0.0662 0.6730 0.4558 0.026 Uiso 1 1 calc R . .
C3 C 0.3337(2) 0.57370(18) 0.44496(15) 0.0253(4) Uani 1 1 d . . .
H3A H 0.3466 0.5517 0.3723 0.030 Uiso 1 1 calc R . .
H3B H 0.2467 0.5060 0.4488 0.030 Uiso 1 1 calc R . .
C4 C 0.4781(2) 0.56668(18) 0.51678(15) 0.0256(4) Uani 1 1 d . . .
H4A H 0.4621 0.5809 0.5886 0.031 Uiso 1 1 calc R . .
H4B H 0.5634 0.6392 0.5175 0.031 Uiso 1 1 calc R . .
C5 C -0.1555(2) 0.86423(19) 0.66536(15) 0.0272(4) Uani 1 1 d . . .
H5A H -0.2496 0.8256 0.6153 0.033 Uiso 1 1 calc R . .
C6 C 0.0660(2) 0.97776(19) 0.73564(14) 0.0239(4) Uani 1 1 d . . .
H6A H 0.1639 1.0357 0.7498 0.029 Uiso 1 1 calc R . .
C7 C 0.1021(2) 0.9065(2) 0.90069(15) 0.0301(5) Uani 1 1 d . . .
H7A H 0.2008 0.9731 0.9218 0.036 Uiso 1 1 calc R . .
H7B H 0.1251 0.8169 0.8909 0.036 Uiso 1 1 calc R . .
C8 C 0.0163(2) 0.93105(18) 0.98703(14) 0.0248(4) Uani 1 1 d . . .
H8A H -0.0820 0.8639 0.9660 0.030 Uiso 1 1 calc R . .
H8B H 0.0774 0.9183 1.0505 0.030 Uiso 1 1 calc R . .
C9 C -0.2788(2) 0.74146(18) 0.35021(15) 0.0225(4) Uani 1 1 d . . .
C10 C 0.7098(2) 0.6407(2) 1.03526(16) 0.0323(5) Uani 1 1 d . . .
H10A H 0.7222 0.6344 1.1048 0.039 Uiso 1 1 calc R . .
C11 C 0.7426(2) 0.62222(17) 0.88378(15) 0.0220(4) Uani 1 1 d . . .
H11A H 0.7793 0.6022 0.8217 0.026 Uiso 1 1 calc R . .
C12 C 0.8536(2) 1.23041(19) 0.79982(15) 0.0277(4) Uani 1 1 d . . .
H12A H 0.9414 1.2440 0.7713 0.033 Uiso 1 1 calc R . .
C13 C 0.7050(2) 1.25684(18) 0.90086(15) 0.0233(4) Uani 1 1 d . . .
H13A H 0.6601 1.2895 0.9572 0.028 Uiso 1 1 calc R . .
C14 C 0.5335(2) 0.72879(18) 0.81963(15) 0.0266(4) Uani 1 1 d . . .
H14A H 0.4247 0.6831 0.8079 0.032 Uiso 1 1 calc R . .
H14B H 0.5648 0.7056 0.7524 0.032 Uiso 1 1 calc R . .
C15 C 0.5485(2) 0.87827(18) 0.85535(15) 0.0249(4) Uani 1 1 d . . .
H15A H 0.6582 0.9242 0.8787 0.030 Uiso 1 1 calc R . .
H15B H 0.4993 0.9007 0.9149 0.030 Uiso 1 1 calc R . .
C16 C 0.4718(2) 0.92494(18) 0.76578(15) 0.0259(4) Uani 1 1 d . . .
H16A H 0.5205 0.8999 0.7064 0.031 Uiso 1 1 calc R . .
H16B H 0.3626 0.8774 0.7429 0.031 Uiso 1 1 calc R . .
C17 C 0.4808(2) 1.07438(18) 0.79268(17) 0.0288(4) Uani 1 1 d . . .
H17A H 0.4224 1.0956 0.7323 0.035 Uiso 1 1 calc R . .
H17B H 0.4321 1.1000 0.8520 0.035 Uiso 1 1 calc R . .
C18 C 1.0863(2) 0.56514(18) 0.78345(15) 0.0237(4) Uani 1 1 d . . .
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate
(isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N7 2.1849(17) 2_576 ?
Mn1 N7 2.1849(17) . ?
Mn1 N6 2.2718(16) . ?
Mn1 N6 2.2718(16) 2_576 ?
Mn1 N3 2.2960(14) 2_576 ?
Mn1 N3 2.2960(15) . ?
Mn2 N14 2.2128(17) 2_767 ?
Mn2 N14 2.2128(17) . ?
Mn2 N10 2.2472(15) 2_767 ?
Mn2 N10 2.2472(15) . ?
Mn2 N13 2.2550(16) 2_777 ?
Mn2 N13 2.2550(16) 1_545 ?
S1 C9 1.630(2) . ?
S2 C18 1.629(2) . ?
N1 C2 1.333(2) . ?
N1 N2 1.360(2) . ?
N1 C3 1.471(2) . ?
N2 C1 1.318(2) . ?
N3 C2 1.330(2) . ?
N3 C1 1.358(2) . ?
N4 C6 1.328(2) . ?
N4 N5 1.361(2) . ?
N4 C7 1.468(2) . ?
N5 C5 1.316(2) . ?
N6 C6 1.323(2) . ?
N6 C5 1.354(2) . ?
N7 C9 1.163(2) . ?
N8 C11 1.323(2) . ?
N8 N9 1.358(2) . ?
N8 C14 1.458(2) . ?
N9 C10 1.317(3) . ?
N10 C11 1.329(2) . ?
N10 C10 1.355(2) . ?
N11 C13 1.323(2) . ?
N11 N12 1.362(2) . ?
N11 C17 1.456(2) . ?
N12 C12 1.315(3) . ?
N13 C13 1.328(2) . ?
N13 C12 1.359(2) . ?
N13 Mn2 2.2550(15) 1_565 ?
N14 C18 1.166(2) . ?
C1 H1A 0.9500 . ?
C2 H2A 0.9500 . ?
C3 C4 1.516(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C4 1.520(3) 2_666 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 C8 1.514(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C8 1.511(4) 2_577 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C15 1.514(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.522(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.520(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
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
N7 Mn1 N7 180.0 2_576 . ?
N7 Mn1 N6 89.92(6) 2_576 . ?
N7 Mn1 N6 90.08(6) . . ?
N7 Mn1 N6 90.08(6) 2_576 2_576 ?
N7 Mn1 N6 89.92(6) . 2_576 ?
N6 Mn1 N6 180.0 . 2_576 ?
N7 Mn1 N3 89.98(6) 2_576 2_576 ?
N7 Mn1 N3 90.02(6) . 2_576 ?
N6 Mn1 N3 91.30(5) . 2_576 ?
N6 Mn1 N3 88.70(5) 2_576 2_576 ?
N7 Mn1 N3 90.02(6) 2_576 . ?
N7 Mn1 N3 89.98(6) . . ?
N6 Mn1 N3 88.70(5) . . ?
N6 Mn1 N3 91.30(5) 2_576 . ?
N3 Mn1 N3 180.000(1) 2_576 . ?
N14 Mn2 N14 180.000(1) 2_767 . ?
N14 Mn2 N10 90.75(6) 2_767 2_767 ?
N14 Mn2 N10 89.25(6) . 2_767 ?
N14 Mn2 N10 89.25(6) 2_767 . ?
N14 Mn2 N10 90.75(6) . . ?
N10 Mn2 N10 180.000(1) 2_767 . ?
N14 Mn2 N13 87.84(6) 2_767 2_777 ?
N14 Mn2 N13 92.16(6) . 2_777 ?
N10 Mn2 N13 86.35(6) 2_767 2_777 ?
N10 Mn2 N13 93.65(6) . 2_777 ?
N14 Mn2 N13 92.16(6) 2_767 1_545 ?
N14 Mn2 N13 87.84(6) . 1_545 ?
N10 Mn2 N13 93.65(6) 2_767 1_545 ?
N10 Mn2 N13 86.35(6) . 1_545 ?
N13 Mn2 N13 180.0 2_777 1_545 ?
C2 N1 N2 109.87(14) . . ?
C2 N1 C3 128.80(15) . . ?
N2 N1 C3 121.11(14) . . ?
C1 N2 N1 102.50(14) . . ?
C2 N3 C1 102.67(15) . . ?
C2 N3 Mn1 132.49(12) . . ?
C1 N3 Mn1 124.79(12) . . ?
C6 N4 N5 109.71(15) . . ?
C6 N4 C7 128.15(16) . . ?
N5 N4 C7 121.61(15) . . ?
C5 N5 N4 102.13(15) . . ?
C6 N6 C5 102.38(16) . . ?
C6 N6 Mn1 125.13(12) . . ?
C5 N6 Mn1 131.38(13) . . ?
C9 N7 Mn1 174.19(16) . . ?
C11 N8 N9 110.10(15) . . ?
C11 N8 C14 128.44(16) . . ?
N9 N8 C14 121.45(15) . . ?
C10 N9 N8 102.42(15) . . ?
C11 N10 C10 102.69(15) . . ?
C11 N10 Mn2 126.45(12) . . ?
C10 N10 Mn2 130.86(13) . . ?
C13 N11 N12 109.94(15) . . ?
C13 N11 C17 128.65(17) . . ?
N12 N11 C17 120.97(16) . . ?
C12 N12 N11 102.30(15) . . ?
C13 N13 C12 102.36(16) . . ?
C13 N13 Mn2 125.50(13) . 1_565 ?
C12 N13 Mn2 131.63(13) . 1_565 ?
C18 N14 Mn2 168.81(15) . . ?
N2 C1 N3 114.78(17) . . ?
N2 C1 H1A 122.6 . . ?
N3 C1 H1A 122.6 . . ?
N3 C2 N1 110.17(16) . . ?
N3 C2 H2A 124.9 . . ?
N1 C2 H2A 124.9 . . ?
N1 C3 C4 112.64(15) . . ?
N1 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
N1 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C4 112.12(19) . 2_666 ?
C3 C4 H4A 109.2 . . ?
C4 C4 H4A 109.2 2_666 . ?
C3 C4 H4B 109.2 . . ?
C4 C4 H4B 109.2 2_666 . ?
H4A C4 H4B 107.9 . . ?
N5 C5 N6 115.14(17) . . ?
N5 C5 H5A 122.4 . . ?
N6 C5 H5A 122.4 . . ?
N6 C6 N4 110.64(16) . . ?
N6 C6 H6A 124.7 . . ?
N4 C6 H6A 124.7 . . ?
N4 C7 C8 112.90(16) . . ?
N4 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
N4 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C8 C8 C7 113.4(2) 2_577 . ?
C8 C8 H8A 108.9 2_577 . ?
C7 C8 H8A 108.9 . . ?
C8 C8 H8B 108.9 2_577 . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
N7 C9 S1 177.93(17) . . ?
N9 C10 N10 114.58(18) . . ?
N9 C10 H10A 122.7 . . ?
N10 C10 H10A 122.7 . . ?
N8 C11 N10 110.21(16) . . ?
N8 C11 H11A 124.9 . . ?
N10 C11 H11A 124.9 . . ?
N12 C12 N13 114.87(17) . . ?
N12 C12 H12A 122.6 . . ?
N13 C12 H12A 122.6 . . ?
N11 C13 N13 110.52(17) . . ?
N11 C13 H13A 124.7 . . ?
N13 C13 H13A 124.7 . . ?
N8 C14 C15 112.28(15) . . ?
N8 C14 H14A 109.1 . . ?
C15 C14 H14A 109.1 . . ?
N8 C14 H14B 109.1 . . ?
C15 C14 H14B 109.1 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 C16 109.48(15) . . ?
C14 C15 H15A 109.8 . . ?
C16 C15 H15A 109.8 . . ?
C14 C15 H15B 109.8 . . ?
C16 C15 H15B 109.8 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 C15 114.08(16) . . ?
C17 C16 H16A 108.7 . . ?
C15 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C15 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
N11 C17 C16 112.61(15) . . ?
N11 C17 H17A 109.1 . . ?
C16 C17 H17A 109.1 . . ?
N11 C17 H17B 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
N14 C18 S2 178.11(18) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 N2 C1 0.5(2) . . . . ?
C3 N1 N2 C1 175.59(16) . . . . ?
N7 Mn1 N3 C2 160.67(17) 2_576 . . . ?
N7 Mn1 N3 C2 -19.33(17) . . . . ?
N6 Mn1 N3 C2 70.76(17) . . . . ?
N6 Mn1 N3 C2 -109.24(17) 2_576 . . . ?
N7 Mn1 N3 C1 -22.43(15) 2_576 . . . ?
N7 Mn1 N3 C1 157.57(15) . . . . ?
N6 Mn1 N3 C1 -112.34(15) . . . . ?
N6 Mn1 N3 C1 67.66(15) 2_576 . . . ?
C6 N4 N5 C5 -0.3(2) . . . . ?
C7 N4 N5 C5 -172.61(16) . . . . ?
N7 Mn1 N6 C6 -27.83(15) 2_576 . . . ?
N7 Mn1 N6 C6 152.17(15) . . . . ?
N3 Mn1 N6 C6 -117.81(15) 2_576 . . . ?
N3 Mn1 N6 C6 62.19(15) . . . . ?
N7 Mn1 N6 C5 166.41(17) 2_576 . . . ?
N7 Mn1 N6 C5 -13.59(17) . . . . ?
N3 Mn1 N6 C5 76.43(17) 2_576 . . . ?
N3 Mn1 N6 C5 -103.57(17) . . . . ?
C11 N8 N9 C10 -0.2(2) . . . . ?
C14 N8 N9 C10 -179.53(17) . . . . ?
N14 Mn2 N10 C11 -163.55(15) 2_767 . . . ?
N14 Mn2 N10 C11 16.45(15) . . . . ?
N13 Mn2 N10 C11 108.66(15) 2_777 . . . ?
N13 Mn2 N10 C11 -71.34(15) 1_545 . . . ?
N14 Mn2 N10 C10 17.41(18) 2_767 . . . ?
N14 Mn2 N10 C10 -162.59(18) . . . . ?
N13 Mn2 N10 C10 -70.37(18) 2_777 . . . ?
N13 Mn2 N10 C10 109.63(18) 1_545 . . . ?
C13 N11 N12 C12 0.4(2) . . . . ?
C17 N11 N12 C12 173.45(16) . . . . ?
N10 Mn2 N14 C18 156.9(8) 2_767 . . . ?
N10 Mn2 N14 C18 -23.1(8) . . . . ?
N13 Mn2 N14 C18 -116.8(8) 2_777 . . . ?
N13 Mn2 N14 C18 63.2(8) 1_545 . . . ?
N1 N2 C1 N3 -0.2(2) . . . . ?
C2 N3 C1 N2 -0.1(2) . . . . ?
Mn1 N3 C1 N2 -177.75(12) . . . . ?
C1 N3 C2 N1 0.4(2) . . . . ?
Mn1 N3 C2 N1 177.80(12) . . . . ?
N2 N1 C2 N3 -0.6(2) . . . . ?
C3 N1 C2 N3 -175.20(17) . . . . ?
C2 N1 C3 C4 -141.12(19) . . . . ?
N2 N1 C3 C4 44.8(2) . . . . ?
N1 C3 C4 C4 -175.3(2) . . . 2_666 ?
N4 N5 C5 N6 0.4(2) . . . . ?
C6 N6 C5 N5 -0.2(2) . . . . ?
Mn1 N6 C5 N5 167.87(13) . . . . ?
C5 N6 C6 N4 0.0(2) . . . . ?
Mn1 N6 C6 N4 -169.11(11) . . . . ?
N5 N4 C6 N6 0.2(2) . . . . ?
C7 N4 C6 N6 171.84(17) . . . . ?
C6 N4 C7 C8 134.41(19) . . . . ?
N5 N4 C7 C8 -54.9(2) . . . . ?
N4 C7 C8 C8 -62.2(3) . . . 2_577 ?
N8 N9 C10 N10 0.6(2) . . . . ?
C11 N10 C10 N9 -0.7(2) . . . . ?
Mn2 N10 C10 N9 178.47(14) . . . . ?
N9 N8 C11 N10 -0.2(2) . . . . ?
C14 N8 C11 N10 179.02(16) . . . . ?
C10 N10 C11 N8 0.5(2) . . . . ?
Mn2 N10 C11 N8 -178.71(11) . . . . ?
N11 N12 C12 N13 0.3(2) . . . . ?
C13 N13 C12 N12 -0.8(2) . . . . ?
Mn2 N13 C12 N12 -172.75(13) 1_565 . . . ?
N12 N11 C13 N13 -0.9(2) . . . . ?
C17 N11 C13 N13 -173.31(17) . . . . ?
C12 N13 C13 N11 1.0(2) . . . . ?
Mn2 N13 C13 N11 173.63(11) 1_565 . . . ?
C11 N8 C14 C15 -117.4(2) . . . . ?
N9 N8 C14 C15 61.7(2) . . . . ?
N8 C14 C15 C16 169.91(16) . . . . ?
C14 C15 C16 C17 -179.62(16) . . . . ?
C13 N11 C17 C16 -131.7(2) . . . . ?
N12 N11 C17 C16 56.7(2) . . . . ?
C15 C16 C17 N11 62.7(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.048
###======

