#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:54:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179134 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/96/4309685.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_4309685
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            'C16 H25 Mn N2 O5 S2'
_chemical_formula_weight         444.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            18
_cell_length_a                   18.1966(7)
_cell_length_b                   18.1966(7)
_cell_length_c                   31.898(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.24
_cell_volume                     9146.9(10)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            19378
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  0.7965
_exptl_absorpt_correction_T_min  0.6195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.525
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0497
_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)+(0.0669P)²+43.8500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                4339
_reflns_number_total             4952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050891hc1_2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_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 

The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'rhomboheral' was replaced with
'rhombohedral' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        9147.0(9)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4309685
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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'
'-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'
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 0.69925(2) 0.87435(2) 0.020647(11) 0.02379(12) Uani 1 1 d . . .
O1 O 0.61017(11) 0.84075(11) -0.01740(6) 0.0304(4) Uani 1 1 d . A .
O2 O 0.72073(10) 0.68870(11) -0.04548(5) 0.0269(3) Uani 1 1 d . . .
O3 O 0.78994(11) 0.88987(11) 0.05785(5) 0.0292(4) Uani 1 1 d . A .
N1 N 0.72554(12) 0.79110(12) -0.00242(6) 0.0227(4) Uani 1 1 d . A .
N2 N 0.79640(12) 0.79113(12) 0.01607(6) 0.0243(4) Uani 1 1 d . . .
C1 C 0.57745(14) 0.77629(15) -0.04406(7) 0.0254(4) Uani 1 1 d . . .
C2 C 0.61379(14) 0.72541(14) -0.05391(7) 0.0242(4) Uani 1 1 d . A .
C3 C 0.57481(16) 0.66033(16) -0.08371(8) 0.0291(5) Uani 1 1 d . . .
H3 H 0.6002 0.6273 -0.0906 0.038(8) Uiso 1 1 calc R A .
C4 C 0.50023(17) 0.64341(18) -0.10324(9) 0.0360(6) Uani 1 1 d . A .
H4 H 0.4741 0.5988 -0.1232 0.050(10) Uiso 1 1 calc R . .
C5 C 0.46413(17) 0.69278(19) -0.09317(9) 0.0380(6) Uani 1 1 d . . .
H5 H 0.4126 0.6813 -0.1063 0.049(10) Uiso 1 1 calc R A .
C6 C 0.50165(16) 0.75820(17) -0.06447(8) 0.0322(5) Uani 1 1 d . A .
H6 H 0.4760 0.7914 -0.0584 0.035(8) Uiso 1 1 calc R . .
C7 C 0.69072(14) 0.73578(14) -0.03343(7) 0.0229(4) Uani 1 1 d . . .
C8 C 0.82434(14) 0.84417(14) 0.04737(7) 0.0251(4) Uani 1 1 d . A .
C9 C 0.89753(16) 0.85313(16) 0.07284(8) 0.0299(5) Uani 1 1 d . . .
H9A H 0.9421 0.9137 0.0736 0.042(9) Uiso 1 1 calc R A .
H9B H 0.9218 0.8215 0.0588 0.034(8) Uiso 1 1 calc R . .
C10 C 0.87342(18) 0.82044(18) 0.11809(8) 0.0344(5) Uani 1 1 d . A .
H10 H 0.8520 0.8548 0.1326 0.033(8) Uiso 1 1 calc R . .
C11 C 0.8043(3) 0.7277(2) 0.11965(11) 0.0563(9) Uani 1 1 d . . .
H11A H 0.8269 0.6923 0.1091 0.102(19) Uiso 1 1 calc R A .
H11B H 0.7564 0.7192 0.1022 0.077(14) Uiso 1 1 calc R . .
H11C H 0.7853 0.7117 0.1487 0.061(11) Uiso 1 1 calc R . .
C12 C 0.9528(3) 0.8337(4) 0.14087(11) 0.0700(13) Uani 1 1 d . . .
H12A H 0.9376 0.8098 0.1692 0.067(12) Uiso 1 1 calc R A .
H12B H 0.9938 0.8946 0.1427 0.080(16) Uiso 1 1 calc R . .
H12C H 0.9781 0.8053 0.1254 0.100(18) Uiso 1 1 calc R . .
S1 S 0.59750(16) 0.7825(2) 0.11528(5) 0.0757(8) Uani 0.630(6) 1 d P A 1
O4 O 0.6059(9) 0.7930(10) 0.0678(4) 0.043(3) Uani 0.630(6) 1 d P A 1
C13 C 0.4947(4) 0.7494(5) 0.12844(19) 0.0593(18) Uani 0.630(6) 1 d P A 1
H13A H 0.4751 0.7829 0.1130 0.089 Uiso 0.630(6) 1 calc PR A 1
H13B H 0.4910 0.7569 0.1586 0.089 Uiso 0.630(6) 1 calc PR A 1
H13C H 0.4591 0.6893 0.1212 0.089 Uiso 0.630(6) 1 calc PR A 1
C14 C 0.6391(6) 0.8834(5) 0.1380(2) 0.103(4) Uani 0.630(6) 1 d P A 1
H14A H 0.7012 0.9136 0.1359 0.155 Uiso 0.630(6) 1 calc PR A 1
H14B H 0.6224 0.8775 0.1675 0.155 Uiso 0.630(6) 1 calc PR A 1
H14C H 0.6171 0.9155 0.1231 0.155 Uiso 0.630(6) 1 calc PR A 1
S12 S 0.59936(16) 0.8261(2) 0.11045(8) 0.0462(9) Uani 0.370(6) 1 d P A 2
O42 O 0.5981(15) 0.7920(18) 0.0692(7) 0.035(4) Uiso 0.370(6) 1 d P A 2
C132 C 0.505(3) 0.748(4) 0.1345(15) 0.29(3) Uiso 0.370(6) 1 d P A 2
H13D H 0.4567 0.7343 0.1160 0.439 Uiso 0.370(6) 1 calc PR A 2
H13E H 0.4969 0.7702 0.1611 0.439 Uiso 0.370(6) 1 calc PR A 2
H13F H 0.5086 0.6972 0.1397 0.439 Uiso 0.370(6) 1 calc PR A 2
C142 C 0.6324(6) 0.7491(6) 0.1436(3) 0.048(2) Uiso 0.370(6) 1 d P A 2
H14D H 0.5948 0.6898 0.1356 0.073 Uiso 0.370(6) 1 calc PR A 2
H14E H 0.6268 0.7558 0.1737 0.073 Uiso 0.370(6) 1 calc PR A 2
H14F H 0.6913 0.7653 0.1372 0.073 Uiso 0.370(6) 1 calc PR A 2
S1S S 0.47070(6) 0.53751(5) 0.05391(2) 0.0488(2) Uani 1 1 d . . .
O1S O 0.45342(16) 0.54961(17) 0.09875(7) 0.0565(6) Uani 1 1 d . . .
C1S C 0.5825(2) 0.5971(2) 0.04733(11) 0.0529(8) Uani 1 1 d . . .
H1S1 H 0.6032 0.6562 0.0555 0.079 Uiso 1 1 calc R . .
H1S2 H 0.5966 0.5951 0.0179 0.079 Uiso 1 1 calc R . .
H1S3 H 0.6093 0.5731 0.0650 0.079 Uiso 1 1 calc R . .
C2S C 0.4434(3) 0.6018(3) 0.02256(12) 0.0623(10) Uani 1 1 d . . .
H2S1 H 0.3819 0.5791 0.0239 0.093 Uiso 1 1 calc R . .
H2S2 H 0.4602 0.6012 -0.0066 0.093 Uiso 1 1 calc R . .
H2S3 H 0.4729 0.6601 0.0332 0.093 Uiso 1 1 calc R . .
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'
Mn Mn 0.3368 0.7283 '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'
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
O1 Mn1 O3 169.78(7) . . ?
O1 Mn1 N1 90.59(8) . . ?
O3 Mn1 N1 79.75(7) . . ?
O1 Mn1 O2 95.76(7) . 11_565 ?
O3 Mn1 O2 94.11(7) . 11_565 ?
N1 Mn1 O2 172.48(8) . 11_565 ?
O1 Mn1 O4 88.4(4) . . ?
O3 Mn1 O4 89.7(4) . . ?
N1 Mn1 O4 98.2(4) . . ?
O2 Mn1 O4 86.0(4) 11_565 . ?
O1 Mn1 O42 86.7(6) . . ?
O3 Mn1 O42 91.6(5) . . ?
N1 Mn1 O42 100.1(7) . . ?
O2 Mn1 O42 84.3(7) 11_565 . ?
O4 Mn1 O42 2.5(9) . . ?
O1 Mn1 N2 94.56(8) . 11_565 ?
O3 Mn1 N2 90.72(7) . 11_565 ?
N1 Mn1 N2 101.77(7) . 11_565 ?
O2 Mn1 N2 73.78(7) 11_565 11_565 ?
O4 Mn1 N2 159.8(4) . 11_565 ?
O42 Mn1 N2 158.0(7) . 11_565 ?
C1 O1 Mn1 129.78(15) . . ?
C7 O2 Mn1 121.56(14) . 12_655 ?
C8 O3 Mn1 113.21(14) . . ?
C7 N1 N2 113.60(18) . . ?
C7 N1 Mn1 131.54(16) . . ?
N2 N1 Mn1 114.82(14) . . ?
C8 N2 N1 109.71(18) . . ?
C8 N2 Mn1 141.42(16) . 12_655 ?
N1 N2 Mn1 108.85(13) . 12_655 ?
O1 C1 C6 117.3(2) . . ?
O1 C1 C2 124.8(2) . . ?
C6 C1 C2 117.9(2) . . ?
C3 C2 C1 119.9(2) . . ?
C3 C2 C7 117.2(2) . . ?
C1 C2 C7 122.9(2) . . ?
C4 C3 C2 121.3(2) . . ?
C3 C4 C5 118.8(2) . . ?
C6 C5 C4 121.4(2) . . ?
C5 C6 C1 120.8(2) . . ?
O2 C7 N1 122.0(2) . . ?
O2 C7 C2 118.5(2) . . ?
N1 C7 C2 119.5(2) . . ?
N2 C8 O3 122.2(2) . . ?
N2 C8 C9 119.5(2) . . ?
O3 C8 C9 118.3(2) . . ?
C8 C9 C10 113.6(2) . . ?
C11 C10 C12 110.6(3) . . ?
C11 C10 C9 112.2(2) . . ?
C12 C10 C9 108.7(2) . . ?
O4 S1 C13 108.2(6) . . ?
O4 S1 C14 108.3(7) . . ?
C13 S1 C14 95.3(5) . . ?
S1 O4 Mn1 139.5(9) . . ?
O42 S12 C132 104.5(19) . . ?
O42 S12 C142 97.0(10) . . ?
C132 S12 C142 74.4(19) . . ?
S12 O42 Mn1 119.8(16) . . ?
O1S S1S C1S 106.41(16) . . ?
O1S S1S C2S 106.83(18) . . ?
C1S S1S C2S 98.19(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
Mn1 O1 1.8662(18) . ?
Mn1 O3 1.9352(17) . ?
Mn1 N1 1.9468(19) . ?
Mn1 O2 1.9732(16) 11_565 ?
Mn1 O4 2.197(12) . ?
Mn1 O42 2.30(2) . ?
Mn1 N2 2.303(2) 11_565 ?
O1 C1 1.325(3) . ?
O2 C7 1.284(3) . ?
O2 Mn1 1.9732(16) 12_655 ?
O3 C8 1.310(3) . ?
N1 C7 1.325(3) . ?
N1 N2 1.418(3) . ?
N2 C8 1.302(3) . ?
N2 Mn1 2.303(2) 12_655 ?
C1 C6 1.407(3) . ?
C1 C2 1.416(3) . ?
C2 C3 1.403(3) . ?
C2 C7 1.469(3) . ?
C3 C4 1.381(3) . ?
C4 C5 1.390(4) . ?
C5 C6 1.382(4) . ?
C8 C9 1.498(3) . ?
C9 C10 1.539(4) . ?
C10 C11 1.520(4) . ?
C10 C12 1.525(4) . ?
S1 O4 1.525(13) . ?
S1 C13 1.706(6) . ?
S1 C14 1.755(8) . ?
S12 O42 1.45(3) . ?
S12 C132 1.76(5) . ?
S12 C142 2.070(10) . ?
S1S O1S 1.504(2) . ?
S1S C1S 1.775(4) . ?
S1S C2S 1.788(4) . ?
