#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013777.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_7013777
loop_
_publ_author_name
'Mossin, Susanne'
'Weihe, Høgni'
'Sørensen, Henning Osholm'
'Lima, Nicola'
'Sessoli, Roberta'
_publ_section_title
;
 Rationalisation of weak ferromagnetism in manganese(III) chains: the
 relation between structure and ordering phenomena.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              632
_journal_page_last               639
_journal_paper_doi               10.1039/b314355d
_journal_year                    2004
_chemical_formula_moiety
;
C11 H25 Mn N4 O2, C F3 O3 S, Cl O4
;
_chemical_formula_sum            'C12 H25 Cl F3 Mn N4 O9 S'
_chemical_formula_weight         548.81
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.169(2)
_cell_length_b                   12.744(3)
_cell_length_c                   16.181(3)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      22.81
_cell_measurement_theta_min      5.69
_cell_volume                     2097.0(8)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
EvalCCD (Duisenberg, 2003) and DREAD (Blessing, 1987)
;
_computing_molecular_graphics    'Ortep II (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      122(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω and φ 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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80396
_diffrn_reflns_theta_full        35.03
_diffrn_reflns_theta_max         35.03
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0244P)²+1.0219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                3894
_reflns_number_total             4785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b314355d.txt
_cod_data_source_block           2
_cod_database_code               7013777
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.0000 0.0000 0.5000 0.00971(4) Uani 1 2 d S . .
C1 C -0.32469(12) -0.03465(10) 0.47004(9) 0.0253(2) Uani 1 1 d . . .
H1A H -0.3413(18) 0.0366(15) 0.4588(11) 0.030 Uiso 1 1 d . . .
H1B H -0.4044(19) -0.0691(15) 0.4681(11) 0.030 Uiso 1 1 d . . .
C2 C -0.23513(12) -0.07937(9) 0.40382(8) 0.0221(2) Uani 1 1 d . . .
H2A H -0.2798(18) -0.0767(13) 0.3502(11) 0.027 Uiso 1 1 d . . .
H2B H -0.2122(18) -0.1500(14) 0.4151(11) 0.027 Uiso 1 1 d . . .
N1 N -0.11084(10) -0.01892(7) 0.39543(6) 0.01547(15) Uani 1 1 d . . .
H1N H -0.1279(16) 0.0373(13) 0.3796(10) 0.019 Uiso 1 1 d . . .
C3 C -0.02053(13) -0.06438(9) 0.33207(7) 0.0212(2) Uani 1 1 d . . .
H3A H -0.0116(17) -0.1380(15) 0.3452(11) 0.025 Uiso 1 1 d . . .
H3B H -0.0606(17) -0.0553(14) 0.2775(10) 0.025 Uiso 1 1 d . . .
C4 C 0.11025(13) -0.00862(9) 0.33863(7) 0.0208(2) Uani 1 1 d . . .
H4A H 0.1025(17) 0.0630(14) 0.3290(10) 0.025 Uiso 1 1 d . . .
H4B H 0.1683(17) -0.0382(14) 0.3000(10) 0.025 Uiso 1 1 d . . .
N2 N 0.15915(9) -0.01979(7) 0.42494(6) 0.01485(15) Uani 1 1 d . . .
H2N H 0.1813(16) -0.0832(13) 0.4314(10) 0.018 Uiso 1 1 d . . .
C5 C 0.27566(11) 0.04741(9) 0.44160(8) 0.0208(2) Uani 1 1 d . . .
H5A H 0.3428(17) 0.0243(14) 0.4031(11) 0.025 Uiso 1 1 d . . .
H5B H 0.2471(17) 0.1166(14) 0.4277(10) 0.025 Uiso 1 1 d . . .
O1 O 0.01065(9) 0.16390(6) 0.48530(5) 0.02037(16) Uani 1 1 d . . .
C6 C -0.01794(14) 0.2500 0.45420(9) 0.0137(2) Uani 1 2 d S . .
H6 H -0.055(2) 0.2500 0.4028(14) 0.016 Uiso 1 2 d S . .
Cl Cl 0.65404(4) 0.2500 0.64990(2) 0.01601(7) Uani 1 2 d S . .
O21 O 0.76717(14) 0.2500 0.59428(9) 0.0279(3) Uani 1 2 d S . .
O22 O 0.69943(17) 0.2500 0.73389(8) 0.0309(3) Uani 1 2 d S . .
O23 O 0.57810(11) 0.15688(8) 0.63464(7) 0.0302(2) Uani 1 1 d . . .
S S 0.71383(4) 0.2500 0.28192(2) 0.01554(7) Uani 1 2 d S . .
O31 O 0.66502(13) 0.2500 0.19848(7) 0.0207(2) Uani 1 2 d S . .
O32 O 0.77883(11) 0.15442(7) 0.30697(6) 0.0283(2) Uani 1 1 d . . .
C31 C 0.5662(2) 0.2500 0.34498(13) 0.0335(4) Uani 1 2 d S . .
F31 F 0.49405(12) 0.16525(11) 0.33009(8) 0.0608(4) Uani 1 1 d . . .
F32 F 0.5965(2) 0.2500 0.42558(9) 0.0543(4) Uani 1 2 d S . .
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'
F F 0.0171 0.0103 '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'
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 Mn N1 85.99(4) . . ?
N1 Mn O1 87.03(4) . 5_556 ?
N2 Mn O1 90.84(3) . . ?
N1 Mn O1 92.97(4) . . ?
C2 C1 C5 115.24(10) . 5_556 ?
C2 C1 H1A 109.5(11) . . ?
C5 C1 H1A 110.0(11) 5_556 . ?
C2 C1 H1B 108.9(12) . . ?
C5 C1 H1B 105.6(12) 5_556 . ?
H1A C1 H1B 107.1(16) . . ?
N1 C2 C1 112.35(9) . . ?
N1 C2 H2A 107.2(11) . . ?
C1 C2 H2A 109.5(11) . . ?
N1 C2 H2B 107.5(11) . . ?
C1 C2 H2B 111.7(11) . . ?
H2A C2 H2B 108.5(15) . . ?
C2 N1 C3 112.62(9) . . ?
C2 N1 Mn 116.98(7) . . ?
C3 N1 Mn 105.93(7) . . ?
C2 N1 H1N 108.4(12) . . ?
C3 N1 H1N 105.6(12) . . ?
Mn N1 H1N 106.6(12) . . ?
N1 C3 C4 108.09(9) . . ?
N1 C3 H3A 106.5(11) . . ?
C4 C3 H3A 111.0(10) . . ?
N1 C3 H3B 108.5(10) . . ?
C4 C3 H3B 112.0(10) . . ?
H3A C3 H3B 110.6(15) . . ?
N2 C4 C3 108.34(9) . . ?
N2 C4 H4A 106.3(11) . . ?
C3 C4 H4A 112.0(11) . . ?
N2 C4 H4B 112.1(10) . . ?
C3 C4 H4B 108.5(11) . . ?
H4A C4 H4B 109.6(15) . . ?
C5 N2 C4 112.40(9) . . ?
C5 N2 Mn 116.96(7) . . ?
C4 N2 Mn 106.36(7) . . ?
C5 N2 H2N 108.4(11) . . ?
C4 N2 H2N 107.3(11) . . ?
Mn N2 H2N 104.8(11) . . ?
N2 C5 C1 111.70(9) . 5_556 ?
N2 C5 H5A 105.6(10) . . ?
C1 C5 H5A 109.9(10) 5_556 . ?
N2 C5 H5B 104.2(11) . . ?
C1 C5 H5B 114.8(10) 5_556 . ?
H5A C5 H5B 110.1(14) . . ?
C6 O1 Mn 155.59(9) . . ?
O1 C6 O1 124.18(14) . 7_565 ?
O1 C6 H6 117.75(11) . . ?
O22 Cl O23 109.60(6) . . ?
O23 Cl O23 111.32(10) . 7_565 ?
O22 Cl O21 109.28(10) . . ?
O23 Cl O21 108.50(6) . . ?
O31 S O32 114.93(5) . . ?
O32 S O32 115.04(9) 7_565 . ?
O31 S C31 104.02(10) . . ?
O32 S C31 102.76(6) . . ?
F31 C31 F31 108.9(2) 7_565 . ?
F31 C31 F32 107.68(13) . . ?
F31 C31 S 110.79(12) . . ?
F32 C31 S 110.92(17) . . ?
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
Mn N2 2.0392(9) . ?
Mn N1 2.0473(9) . ?
Mn O1 2.1051(8) . ?
C1 C2 1.517(2) . ?
C1 C5 1.523(2) 5_556 ?
C1 H1A 0.94(2) . ?
C1 H1B 0.922(19) . ?
C2 N1 1.4864(15) . ?
C2 H2A 0.979(18) . ?
C2 H2B 0.948(18) . ?
N1 C3 1.4934(15) . ?
N1 H1N 0.780(17) . ?
C3 C4 1.5116(18) . ?
C3 H3A 0.966(18) . ?
C3 H3B 0.980(17) . ?
C4 N2 1.4893(15) . ?
C4 H4A 0.929(18) . ?
C4 H4B 0.939(17) . ?
N2 C5 1.4865(15) . ?
N2 H2N 0.845(16) . ?
C5 H5A 0.970(17) . ?
C5 H5B 0.955(18) . ?
O1 C6 1.2417(10) . ?
C6 H6 0.91(2) . ?
Cl O22 1.4354(14) . ?
Cl O23 1.4373(10) . ?
Cl O21 1.4607(13) . ?
S O31 1.4384(12) . ?
S O32 1.4439(9) . ?
S C31 1.815(2) . ?
C31 F31 1.3276(18) . ?
C31 F32 1.340(3) . ?
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
C5 C1 C2 N1 -69.03(13) 5_556 . . . ?
C1 C2 N1 C3 178.32(10) . . . . ?
C1 C2 N1 Mn 55.24(12) . . . . ?
N2 Mn N1 C2 141.62(8) . . . . ?
N2 Mn N1 C2 -38.38(8) 5_556 . . . ?
O1 Mn N1 C2 52.25(8) 5_556 . . . ?
O1 Mn N1 C2 -127.75(8) . . . . ?
N2 Mn N1 C3 15.17(7) . . . . ?
N2 Mn N1 C3 -164.83(7) 5_556 . . . ?
O1 Mn N1 C3 -74.20(7) 5_556 . . . ?
O1 Mn N1 C3 105.80(7) . . . . ?
C2 N1 C3 C4 -170.70(9) . . . . ?
Mn N1 C3 C4 -41.65(10) . . . . ?
N1 C3 C4 N2 56.42(12) . . . . ?
C3 C4 N2 C5 -170.24(9) . . . . ?
C3 C4 N2 Mn -41.04(10) . . . . ?
N1 Mn N2 C5 -39.29(8) 5_556 . . . ?
N1 Mn N2 C5 140.71(8) . . . . ?
O1 Mn N2 C5 -132.21(8) 5_556 . . . ?
O1 Mn N2 C5 47.79(8) . . . . ?
N1 Mn N2 C4 -165.80(7) 5_556 . . . ?
N1 Mn N2 C4 14.20(7) . . . . ?
O1 Mn N2 C4 101.28(7) 5_556 . . . ?
O1 Mn N2 C4 -78.72(7) . . . . ?
C4 N2 C5 C1 -179.75(9) . . . 5_556 ?
Mn N2 C5 C1 56.78(11) . . . 5_556 ?
N2 Mn O1 C6 95.6(2) . . . . ?
N2 Mn O1 C6 -84.4(2) 5_556 . . . ?
N1 Mn O1 C6 -170.4(2) 5_556 . . . ?
N1 Mn O1 C6 9.6(2) . . . . ?
Mn O1 C6 O1 165.85(8) . . . 7_565 ?
O31 S C31 F31 -60.48(14) . . . 7_565 ?
O32 S C31 F31 59.65(16) 7_565 . . 7_565 ?
O32 S C31 F31 179.40(13) . . . 7_565 ?
O31 S C31 F31 60.48(14) . . . . ?
O32 S C31 F31 -179.40(13) 7_565 . . . ?
O32 S C31 F31 -59.65(15) . . . . ?
O31 S C31 F32 180.0 . . . . ?
O32 S C31 F32 -59.87(5) 7_565 . . . ?
O32 S C31 F32 59.87(5) . . . . ?
