#------------------------------------------------------------------------------
#$Date: 2016-08-06 09:24:30 +0300 (Sat, 06 Aug 2016) $
#$Revision: 185065 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/02/7040205.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_7040205
loop_
_publ_author_name
'Saad, Fawaz A.'
'Knight, James C.'
'Kariuki, Benson M.'
'Amoroso, Angelo J.'
_publ_section_title
;
 Co-ordination behaviour of a novel tristhiourea tripodal ligand;
 structural variations in a series of transition metal complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10280
_journal_page_last               10288
_journal_paper_doi               10.1039/c6dt01148a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C42 H36 Mn N10 O3 S3, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C44 H39 Cl2 Mn N11 O11 S3'
_chemical_formula_weight         1119.88
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-22 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.7370(4)
_cell_length_b                   13.7370(13)
_cell_length_c                   44.1110(15)
_cell_measurement_reflns_used    1324
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.518
_cell_volume                     7208.8(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1933
_diffrn_reflns_av_unetI/netI     0.2751
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            8291
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.518
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.8913
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Denzo/Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             3450
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2831
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0739
_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)+(0.0576P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1324
_reflns_number_total             2831
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01148a2.cif
_cod_data_source_block           aja0907
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        7208.8(5)
_cod_database_code               7040205
_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   0.891
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.6260(4) 0.4080(4) 0.06721(12) 0.0371(12) Uani 1 1 d . . .
H1A H 0.6086 0.3933 0.0458 0.045 Uiso 1 1 calc R U .
H1B H 0.6852 0.4857 0.0694 0.045 Uiso 1 1 calc R U .
C2 C 0.5228(4) 0.3906(4) 0.08399(13) 0.0337(11) Uani 1 1 d . . .
C3 C 0.4396(5) 0.4002(4) 0.06890(13) 0.0422(14) Uani 1 1 d . . .
H3 H 0.4425 0.4110 0.0480 0.051 Uiso 1 1 calc R U .
C4 C 0.3511(4) 0.3930(5) 0.08628(15) 0.0431(14) Uani 1 1 d . . .
H4 H 0.2937 0.3989 0.0769 0.052 Uiso 1 1 calc R U .
C5 C 0.3482(4) 0.3776(4) 0.11670(15) 0.0431(14) Uani 1 1 d . . .
H5 H 0.2896 0.3729 0.1283 0.052 Uiso 1 1 calc R U .
C6 C 0.4347(4) 0.3690(4) 0.12993(12) 0.0283(11) Uani 1 1 d . . .
C7 C 0.4536(3) 0.2911(4) 0.17870(13) 0.0297(11) Uani 1 1 d . . .
C8 C 0.3930(4) 0.3483(4) 0.22532(15) 0.0405(14) Uani 1 1 d . . .
C9 C 0.3722(4) 0.3229(4) 0.25805(15) 0.0398(13) Uani 1 1 d . . .
C10 C 0.3439(4) 0.3906(4) 0.27496(15) 0.0431(14) Uani 1 1 d . . .
H10 H 0.3421 0.4506 0.2658 0.052 Uiso 1 1 calc R U .
C11 C 0.3191(5) 0.3692(5) 0.30476(14) 0.0473(14) Uani 1 1 d . . .
H11 H 0.3015 0.4155 0.3160 0.057 Uiso 1 1 calc R U .
C12 C 0.3196(5) 0.2789(5) 0.31868(15) 0.0525(16) Uani 1 1 d . . .
H12 H 0.3008 0.2635 0.3391 0.063 Uiso 1 1 calc R U .
C13 C 0.3482(5) 0.2125(5) 0.30204(16) 0.0468(14) Uani 1 1 d . . .
H13 H 0.3510 0.1533 0.3114 0.056 Uiso 1 1 calc R U .
C14 C 0.3728(4) 0.2330(4) 0.27164(14) 0.0419(14) Uani 1 1 d . . .
H14 H 0.3897 0.1863 0.2603 0.050 Uiso 1 1 calc R U .
N1 N 0.6667 0.3333 0.07878(19) 0.0310(17) Uani 1 3 d S T P
N2 N 0.5211(3) 0.3734(3) 0.11396(11) 0.0322(10) Uani 1 1 d . . .
N3 N 0.4346(3) 0.3591(3) 0.16132(11) 0.0340(10) Uani 1 1 d . . .
H3A H 0.4198 0.4043 0.1711 0.041 Uiso 1 1 calc R U .
N4 N 0.4375(3) 0.2917(3) 0.20912(11) 0.0367(10) Uani 1 1 d . . .
H4A H 0.4572 0.2521 0.2198 0.044 Uiso 1 1 calc R U .
S1 S 0.49653(10) 0.20274(10) 0.16514(4) 0.0355(4) Uani 1 1 d . . .
O1 O 0.3722(4) 0.4144(3) 0.21189(10) 0.0542(12) Uani 1 1 d . . .
O2 O 0.6469(3) 0.4210(3) 0.24492(11) 0.0499(11) Uani 1 1 d . . .
O3 O 0.6667 0.3333 0.2882(2) 0.075(3) Uani 1 3 d S T P
O4 O 0.3333 0.6667 -0.0001(3) 0.155(6) Uani 1 3 d S T P
O5 O 0.2331(4) 0.6619(4) 0.03988(17) 0.097(2) Uani 1 1 d . . .
Mn1 Mn 0.6667 0.3333 0.13040(3) 0.0291(4) Uani 1 3 d S T P
Cl1 Cl 0.6667 0.3333 0.25665(7) 0.0481(7) Uani 1 3 d S T P
Cl2 Cl 0.3333 0.6667 0.0302 0.0412(6) Uani 1 3 d S T P
C15 C 0.365(4) 0.739(2) 0.1285(5) 0.164(14) Uani 0.3333 1 d D U P
C16 C 0.3981(18) 0.8118(15) 0.1564(4) 0.065(6) Uani 0.3333 1 d D U P
H16A H 0.4310 0.7849 0.1710 0.097 Uiso 0.3333 1 calc R U P
H16B H 0.3325 0.8089 0.1650 0.097 Uiso 0.3333 1 calc R U P
H16C H 0.4515 0.8880 0.1511 0.097 Uiso 0.3333 1 calc R U P
N5 N 0.3333 0.6667 0.1159(4) 0.1502(13) Uani 1 3 d DS TU P
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'
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'
Mn Mn 0.3368 0.7283 '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'
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
N1 C1 C2 111.8(4) . .
N1 C1 H1A 109.3 . .
C2 C1 H1A 109.3 . .
N1 C1 H1B 109.3 . .
C2 C1 H1B 109.3 . .
H1A C1 H1B 107.9 . .
N2 C2 C3 123.2(5) . .
N2 C2 C1 116.3(4) . .
C3 C2 C1 120.3(5) . .
C2 C3 C4 117.3(5) . .
C2 C3 H3 121.3 . .
C4 C3 H3 121.3 . .
C5 C4 C3 120.7(5) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
C4 C5 C6 118.2(5) . .
C4 C5 H5 120.9 . .
C6 C5 H5 120.9 . .
N2 C6 C5 123.2(5) . .
N2 C6 N3 118.7(4) . .
C5 C6 N3 118.1(5) . .
N3 C7 N4 118.3(4) . .
N3 C7 S1 123.9(4) . .
N4 C7 S1 117.8(4) . .
O1 C8 N4 119.3(6) . .
O1 C8 C9 123.7(5) . .
N4 C8 C9 117.0(5) . .
C14 C9 C10 119.7(6) . .
C14 C9 C8 123.3(5) . .
C10 C9 C8 116.8(5) . .
C11 C10 C9 120.0(6) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
C10 C11 C12 120.7(6) . .
C10 C11 H11 119.6 . .
C12 C11 H11 119.6 . .
C13 C12 C11 119.2(6) . .
C13 C12 H12 120.4 . .
C11 C12 H12 120.4 . .
C12 C13 C14 120.5(6) . .
C12 C13 H13 119.7 . .
C14 C13 H13 119.7 . .
C9 C14 C13 119.8(6) . .
C9 C14 H14 120.1 . .
C13 C14 H14 120.1 . .
C1 N1 C1 108.8(4) 3_665 2_655
C1 N1 C1 108.8(4) 3_665 .
C1 N1 C1 108.8(4) 2_655 .
C1 N1 Mn1 110.2(4) 3_665 .
C1 N1 Mn1 110.2(4) 2_655 .
C1 N1 Mn1 110.1(4) . .
C2 N2 C6 117.3(4) . .
C2 N2 Mn1 112.9(3) . .
C6 N2 Mn1 129.4(3) . .
C7 N3 C6 130.6(4) . .
C7 N3 H3A 114.7 . .
C6 N3 H3A 114.7 . .
C7 N4 C8 128.6(5) . .
C7 N4 H4A 115.7 . .
C8 N4 H4A 115.7 . .
C7 S1 Mn1 103.09(17) . .
N1 Mn1 N2 72.67(11) . 2_655
N1 Mn1 N2 72.68(11) . 3_665
N2 Mn1 N2 111.56(10) 2_655 3_665
N1 Mn1 N2 72.68(11) . .
N2 Mn1 N2 111.53(10) 2_655 .
N2 Mn1 N2 111.51(10) 3_665 .
N1 Mn1 S1 125.89(4) . 2_655
N2 Mn1 S1 77.09(10) 2_655 2_655
N2 Mn1 S1 78.44(10) 3_665 2_655
N2 Mn1 S1 161.41(13) . 2_655
N1 Mn1 S1 125.88(4) . .
N2 Mn1 S1 78.43(10) 2_655 .
N2 Mn1 S1 161.42(13) 3_665 .
N2 Mn1 S1 77.06(10) . .
S1 Mn1 S1 89.13(6) 2_655 .
N1 Mn1 S1 125.87(4) . 3_665
N2 Mn1 S1 161.43(13) 2_655 3_665
N2 Mn1 S1 77.07(10) 3_665 3_665
N2 Mn1 S1 78.40(10) . 3_665
S1 Mn1 S1 89.13(6) 2_655 3_665
S1 Mn1 S1 89.11(6) . 3_665
O3 Cl1 O2 110.8(2) . 3_665
O3 Cl1 O2 110.8(2) . 2_655
O2 Cl1 O2 108.1(2) 3_665 2_655
O3 Cl1 O2 110.8(2) . .
O2 Cl1 O2 108.1(2) 3_665 .
O2 Cl1 O2 108.1(2) 2_655 .
O4 Cl2 O5 107.6(3) . .
O4 Cl2 O5 107.6(3) . 3_565
O5 Cl2 O5 111.3(3) . 3_565
O4 Cl2 O5 107.6(3) . 2_665
O5 Cl2 O5 111.3(3) . 2_665
O5 Cl2 O5 111.3(3) 3_565 2_665
N5 C15 C15 43.3(14) . 3_565
N5 C15 C15 43.3(14) . 2_665
C15 C15 C15 60.001(7) 3_565 2_665
N5 C15 C16 158(3) . .
C15 C15 C16 120(3) 3_565 .
C15 C15 C16 120(3) 2_665 .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 N5 C15 93(3) . 2_665
C15 N5 C15 93(3) . 3_565
C15 N5 C15 93(3) 2_665 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.483(6) .
C1 C2 1.510(7) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N2 1.341(7) .
C2 C3 1.384(7) .
C3 C4 1.398(8) .
C3 H3 0.9300 .
C4 C5 1.356(9) .
C4 H4 0.9300 .
C5 C6 1.380(7) .
C5 H5 0.9300 .
C6 N2 1.355(6) .
C6 N3 1.391(6) .
C7 N3 1.331(6) .
C7 N4 1.360(7) .
C7 S1 1.702(5) .
C8 O1 1.231(6) .
C8 N4 1.401(7) .
C8 C9 1.479(8) .
C9 C14 1.376(7) .
C9 C10 1.390(7) .
C10 C11 1.353(8) .
C10 H10 0.9300 .
C11 C12 1.388(8) .
C11 H11 0.9300 .
C12 C13 1.371(8) .
C12 H12 0.9300 .
C13 C14 1.377(8) .
C13 H13 0.9300 .
C14 H14 0.9300 .
N1 C1 1.482(6) 3_665
N1 C1 1.482(6) 2_655
N1 Mn1 2.277(8) .
N2 Mn1 2.436(4) .
N3 H3A 0.8600 .
N4 H4A 0.8600 .
S1 Mn1 2.6148(16) .
O2 Cl1 1.456(4) .
O3 Cl1 1.390(9) .
O4 Cl2 1.335(14) .
O5 Cl2 1.411(5) .
Mn1 N2 2.435(4) 2_655
Mn1 N2 2.435(4) 3_665
Mn1 S1 2.6139(16) 2_655
Mn1 S1 2.6151(16) 3_665
Cl1 O2 1.455(4) 3_665
Cl1 O2 1.455(4) 2_655
Cl2 O5 1.411(5) 3_565
Cl2 O5 1.411(5) 2_665
C15 N5 1.030(9) .
C15 C15 1.50(4) 3_565
C15 C15 1.50(4) 2_665
C15 C16 1.503(9) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
N5 C15 1.030(9) 2_665
N5 C15 1.030(9) 3_565
