#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:54:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179134 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/96/4309687.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_4309687
loop_
_publ_author_name
'Rohith P. John'
'Kyungjae Lee'
'Beom Jin Kim'
'Byoung Jin Suh'
'Hackjune Rhee'
'Myoung Soo Lah'
_publ_section_title
;
Modulation of the Ring Size and Nuclearity of Metallamacrocycles via the
Steric Effect of Ligands: Preparation and Characterization of 18-Membered
Hexanuclear, 24-Membered Octanuclear, and 30-Membered Decanuclear Manganese
Metalladiazamacrocycles with α- and β-Branched N-Acylsalicylhydrazides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7109
_journal_page_last               7121
_journal_paper_doi               10.1021/ic050891h
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C17 H27 Mn N2 O5 S2'
_chemical_formula_weight         458.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            36
_cell_length_a                   18.4008(16)
_cell_length_b                   18.4008(16)
_cell_length_c                   64.805(11)
_cell_measurement_reflns_used    6732
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.21
_cell_volume                     19003(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  WinGX
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -86
_diffrn_reflns_number            38002
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.8152
_exptl_absorpt_correction_T_min  0.7841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8640
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5202
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0664P)²+62.7775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                3984
_reflns_number_total             5202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050891hc1_4.cif
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4309687
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Mn1A Mn 0.70248(2) 0.87848(2) 0.989951(5) 0.02988(12) Uani 1 1 d . . .
O1A O 0.61355(11) 0.84453(12) 1.00842(3) 0.0382(4) Uani 1 1 d . A .
O2A O 0.72043(11) 0.69164(11) 1.02183(3) 0.0331(4) Uani 1 1 d . . .
O3A O 0.79158(12) 0.89354(11) 0.97163(3) 0.0370(4) Uani 1 1 d . A .
N1A N 0.72757(12) 0.79522(12) 1.00111(3) 0.0281(4) Uani 1 1 d . A .
N2A N 0.79736(12) 0.79482(12) 0.99194(3) 0.0294(4) Uani 1 1 d . . .
C1A C 0.57985(15) 0.77946(16) 1.02109(4) 0.0325(5) Uani 1 1 d . . .
C2A C 0.61460(14) 0.72807(15) 1.02568(4) 0.0298(5) Uani 1 1 d . A .
C3A C 0.57428(16) 0.66202(16) 1.03991(4) 0.0347(5) Uani 1 1 d . . .
H3A H 0.5984 0.6282 1.0431 0.042 Uiso 1 1 calc R A .
C4A C 0.50061(18) 0.64545(18) 1.04936(4) 0.0426(6) Uani 1 1 d . A .
H4A H 0.4734 0.6000 1.0587 0.051 Uiso 1 1 calc R . .
C5A C 0.46675(17) 0.69619(18) 1.04494(5) 0.0442(6) Uani 1 1 d . . .
H5A H 0.4163 0.6856 1.0516 0.053 Uiso 1 1 calc R A .
C6A C 0.50476(17) 0.76132(18) 1.03122(4) 0.0407(6) Uani 1 1 d . A .
H6A H 0.4800 0.7949 1.0285 0.049 Uiso 1 1 calc R . .
C7A C 0.69146(14) 0.73887(14) 1.01597(3) 0.0276(4) Uani 1 1 d . . .
C8A C 0.82448(16) 0.84702(15) 0.97635(4) 0.0331(5) Uani 1 1 d . A .
C9A C 0.89192(18) 0.84953(17) 0.96295(4) 0.0393(6) Uani 1 1 d . . .
H9A1 H 0.9204 0.8241 0.9705 0.047 Uiso 1 1 calc R A .
H9A2 H 0.9341 0.9088 0.9601 0.047 Uiso 1 1 calc R . .
C10A C 0.8586(2) 0.80249(18) 0.94205(4) 0.0419(6) Uani 1 1 d . A .
C11A C 0.8475(3) 0.8582(2) 0.92657(4) 0.0600(9) Uani 1 1 d . . .
H11A H 0.9014 0.9096 0.9244 0.090 Uiso 1 1 calc R A .
H11B H 0.8066 0.8728 0.9319 0.090 Uiso 1 1 calc R . .
H11C H 0.8272 0.8282 0.9135 0.090 Uiso 1 1 calc R . .
C12A C 0.9237(2) 0.7819(2) 0.93376(5) 0.0534(8) Uani 1 1 d . . .
H12A H 0.9067 0.7567 0.9200 0.080 Uiso 1 1 calc R A .
H12B H 0.9279 0.7422 0.9431 0.080 Uiso 1 1 calc R . .
H12C H 0.9783 0.8334 0.9328 0.080 Uiso 1 1 calc R . .
C13A C 0.7757(2) 0.7214(2) 0.94530(4) 0.0499(7) Uani 1 1 d . . .
H13A H 0.7590 0.6891 0.9324 0.075 Uiso 1 1 calc R A .
H13B H 0.7324 0.7348 0.9494 0.075 Uiso 1 1 calc R . .
H13C H 0.7823 0.6883 0.9562 0.075 Uiso 1 1 calc R . .
S1S S 0.53319(7) 0.46419(6) 0.026362(15) 0.0644(3) Uani 1 1 d . . .
O1S O 0.55330(19) 0.45475(18) 0.04840(4) 0.0732(7) Uani 1 1 d . . .
C1S C 0.4225(2) 0.4033(2) 0.02383(7) 0.0679(10) Uani 1 1 d . . .
H1S1 H 0.4040 0.3445 0.0269 0.102 Uiso 1 1 calc R . .
H1S2 H 0.4064 0.4081 0.0097 0.102 Uiso 1 1 calc R . .
H1S3 H 0.3960 0.4239 0.0335 0.102 Uiso 1 1 calc R . .
C2S C 0.5599(3) 0.4002(3) 0.01094(7) 0.0835(13) Uani 1 1 d . . .
H2S1 H 0.6205 0.4220 0.0117 0.125 Uiso 1 1 calc R . .
H2S2 H 0.5437 0.4011 -0.0034 0.125 Uiso 1 1 calc R . .
H2S3 H 0.5300 0.3424 0.0161 0.125 Uiso 1 1 calc R . .
S1A S 0.60218(10) 0.78681(12) 0.94433(2) 0.0491(4) Uani 0.710(5) 1 d P A 1
O4A O 0.60596(17) 0.79656(14) 0.96654(4) 0.0648(8) Uani 0.710(5) 1 d P A 1
C14A C 0.4953(3) 0.7449(3) 0.93732(7) 0.0919(16) Uani 0.710(5) 1 d P A 1
H14A H 0.4609 0.6919 0.9446 0.138 Uiso 0.710(5) 1 calc PR A 1
H14B H 0.4891 0.7349 0.9224 0.138 Uiso 0.710(5) 1 calc PR A 1
H14C H 0.4770 0.7848 0.9411 0.138 Uiso 0.710(5) 1 calc PR A 1
C15A C 0.6389(4) 0.8875(3) 0.93318(7) 0.0622(13) Uani 0.710(5) 1 d P A 1
H15A H 0.6028 0.9098 0.9376 0.093 Uiso 0.710(5) 1 calc PR A 1
H15B H 0.6373 0.8828 0.9181 0.093 Uiso 0.710(5) 1 calc PR A 1
H15C H 0.6966 0.9255 0.9377 0.093 Uiso 0.710(5) 1 calc PR A 1
S2A S 0.6098(5) 0.8223(3) 0.94260(8) 0.130(3) Uani 0.290(5) 1 d PD A 2
O42 O 0.60596(17) 0.79656(14) 0.96654(4) 0.0648(8) Uani 0.29 1 d P A 2
C142 C 0.4953(3) 0.7449(3) 0.93732(7) 0.0919(16) Uani 0.29 1 d PD A 2
H14D H 0.4808 0.6901 0.9431 0.138 Uiso 0.290(5) 1 calc PR A 2
H14E H 0.4855 0.7397 0.9224 0.138 Uiso 0.290(5) 1 calc PR A 2
H14F H 0.4604 0.7650 0.9437 0.138 Uiso 0.290(5) 1 calc PR A 2
C152 C 0.6201(8) 0.7512(7) 0.92464(16) 0.0622(13) Uani 0.29 1 d PD A 2
H15D H 0.6786 0.7640 0.9244 0.093 Uiso 0.290(5) 1 calc PR A 2
H15E H 0.6035 0.7585 0.9108 0.093 Uiso 0.290(5) 1 calc PR A 2
H15F H 0.5839 0.6931 0.9291 0.093 Uiso 0.290(5) 1 calc PR A 2
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'
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
O1A Mn1A O3A 169.62(8) . . ?
O1A Mn1A N1A 90.67(8) . . ?
O3A Mn1A N1A 79.79(8) . . ?
O1A Mn1A O2A 94.98(8) . 20_567 ?
O3A Mn1A O2A 94.82(8) . 20_567 ?
N1A Mn1A O2A 173.16(8) . 20_567 ?
O1A Mn1A O4A 86.66(10) . . ?
O3A Mn1A O4A 90.62(10) . . ?
N1A Mn1A O4A 98.15(9) . . ?
O2A Mn1A O4A 86.04(8) 20_567 . ?
O1A Mn1A N2A 95.61(8) . 20_567 ?
O3A Mn1A N2A 90.39(8) . 20_567 ?
N1A Mn1A N2A 101.87(8) . 20_567 ?
O2A Mn1A N2A 73.78(7) 20_567 20_567 ?
O4A Mn1A N2A 159.82(8) . 20_567 ?
C1A O1A Mn1A 129.58(17) . . ?
C7A O2A Mn1A 121.71(15) . 21_657 ?
C8A O3A Mn1A 113.60(15) . . ?
C7A N1A N2A 113.67(19) . . ?
C7A N1A Mn1A 131.49(17) . . ?
N2A N1A Mn1A 114.84(14) . . ?
C8A N2A N1A 109.5(2) . . ?
C8A N2A Mn1A 142.05(17) . 21_657 ?
N1A N2A Mn1A 108.47(13) . 21_657 ?
O1A C1A C6A 117.6(2) . . ?
O1A C1A C2A 124.9(2) . . ?
C6A C1A C2A 117.5(2) . . ?
C3A C2A C1A 119.8(2) . . ?
C3A C2A C7A 117.0(2) . . ?
C1A C2A C7A 123.2(2) . . ?
C4A C3A C2A 121.3(3) . . ?
C3A C4A C5A 118.9(3) . . ?
C6A C5A C4A 121.2(3) . . ?
C5A C6A C1A 121.3(3) . . ?
O2A C7A N1A 122.0(2) . . ?
O2A C7A C2A 118.7(2) . . ?
N1A C7A C2A 119.3(2) . . ?
O3A C8A N2A 122.0(2) . . ?
O3A C8A C9A 119.5(2) . . ?
N2A C8A C9A 118.5(2) . . ?
C8A C9A C10A 113.4(2) . . ?
C11A C10A C12A 108.9(2) . . ?
C11A C10A C13A 110.2(3) . . ?
C12A C10A C13A 109.4(3) . . ?
C11A C10A C9A 110.3(2) . . ?
C12A C10A C9A 107.8(3) . . ?
C13A C10A C9A 110.3(2) . . ?
O1S S1S C1S 106.58(19) . . ?
O1S S1S C2S 106.8(2) . . ?
C1S S1S C2S 98.0(2) . . ?
O4A S1A C14A 106.4(2) . . ?
O4A S1A C15A 107.8(2) . . ?
C14A S1A C15A 96.3(3) . . ?
S1A O4A Mn1A 136.63(18) . . ?
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
Mn1A O1A 1.8651(19) . ?
Mn1A O3A 1.9286(18) . ?
Mn1A N1A 1.947(2) . ?
Mn1A O2A 1.9685(17) 20_567 ?
Mn1A O4A 2.247(2) . ?
Mn1A N2A 2.310(2) 20_567 ?
O1A C1A 1.323(3) . ?
O2A C7A 1.283(3) . ?
O2A Mn1A 1.9685(17) 21_657 ?
O3A C8A 1.308(3) . ?
N1A C7A 1.325(3) . ?
N1A N2A 1.418(3) . ?
N2A C8A 1.309(3) . ?
N2A Mn1A 2.310(2) 21_657 ?
C1A C6A 1.411(4) . ?
C1A C2A 1.413(3) . ?
C2A C3A 1.406(3) . ?
C2A C7A 1.468(3) . ?
C3A C4A 1.375(4) . ?
C4A C5A 1.387(4) . ?
C5A C6A 1.371(4) . ?
C8A C9A 1.496(4) . ?
C9A C10A 1.558(4) . ?
C10A C11A 1.520(4) . ?
C10A C12A 1.523(4) . ?
C10A C13A 1.524(5) . ?
S1S O1S 1.507(3) . ?
S1S C1S 1.774(4) . ?
S1S C2S 1.790(5) . ?
S1A O4A 1.448(3) . ?
S1A C14A 1.775(5) . ?
S1A C15A 1.778(6) . ?
S2A C152 1.830(12) . ?
