#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:21:01 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180035 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/29/7032913.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_7032913
loop_
_publ_author_name
'Han, Song-De'
'Miao, Xiao-Hong'
'Liu, Sui-Jun'
'Bu, Xian-He'
_publ_section_title
;
 A series of cobalt and nickel clusters based on thiol-containing ligands
 accompanied by in situ ligand formation.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              560
_journal_page_last               567
_journal_paper_doi               10.1039/c4dt03109a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C30 H22 N4 Ni3 O2 S10'
_chemical_formula_sum            'C30 H22 N4 Ni3 O2 S10'
_chemical_formula_weight         967.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.89(3)
_cell_angle_beta                 96.17(3)
_cell_angle_gamma                110.77(3)
_cell_formula_units_Z            1
_cell_length_a                   7.6972(15)
_cell_length_b                   9.965(2)
_cell_length_c                   12.372(3)
_cell_measurement_temperature    293(2)
_cell_volume                     874.4(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    DirectMethod
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  SCX-MINI
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7439
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    2.234
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3064
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0536P)²+1.4371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                2652
_reflns_number_total             3071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03109a2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7032912--7032919.cif.
;
_cod_database_code               7032913
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ni1 Ni 1.0000 0.5000 0.5000 0.0283(2) Uani 1 2 d S . .
Ni2 Ni 0.84741(9) 0.52452(7) 0.23219(5) 0.0380(2) Uani 1 1 d . A .
S3 S 1.11656(18) 0.62217(12) 0.36351(9) 0.0377(3) Uani 1 1 d . . .
S4 S 0.79398(19) 0.08249(13) 0.28541(10) 0.0412(3) Uani 1 1 d . . .
S5 S 0.64865(17) 0.32944(14) 0.30815(10) 0.0420(3) Uani 1 1 d . . .
S2 S 1.29031(18) 0.53006(15) 0.29547(10) 0.0460(3) Uani 1 1 d . . .
S1 S 1.21508(19) 0.29502(17) 0.10574(11) 0.0520(4) Uani 1 1 d . . .
N2 N 0.9640(5) 0.3174(4) 0.4201(3) 0.0312(8) Uani 1 1 d . . .
N1 N 0.9716(5) 0.4102(4) 0.1489(3) 0.0353(9) Uani 1 1 d . . .
C2 C 0.8109(6) 0.2535(5) 0.3457(3) 0.0321(10) Uani 1 1 d . . .
C3 C 1.1404(7) 0.4145(5) 0.1827(4) 0.0381(11) Uani 1 1 d . . .
C4 C 1.0025(7) 0.0983(5) 0.3649(3) 0.0329(10) Uani 1 1 d . . .
C5 C 0.9979(7) 0.2314(6) 0.0210(4) 0.0421(12) Uani 1 1 d . . .
O1 O 0.7456(6) 0.6361(5) 0.1904(4) 0.0718(12) Uani 1 1 d . . .
C7 C 0.8851(7) 0.3045(5) 0.0567(4) 0.0368(11) Uani 1 1 d . . .
C8 C 0.7043(8) 0.2680(6) 0.0047(4) 0.0528(14) Uani 1 1 d . . .
H8A H 0.6293 0.3171 0.0277 0.063 Uiso 1 1 calc R . .
C9 C 0.9295(8) 0.1193(6) -0.0680(4) 0.0503(14) Uani 1 1 d . . .
H9A H 1.0048 0.0711 -0.0920 0.060 Uiso 1 1 calc R . .
C10 C 0.7495(9) 0.0840(7) -0.1177(4) 0.0611(16) Uani 1 1 d . . .
H10A H 0.7009 0.0098 -0.1763 0.073 Uiso 1 1 calc R . .
C11 C 0.6354(9) 0.1576(7) -0.0821(5) 0.0681(18) Uani 1 1 d . . .
H11A H 0.5129 0.1317 -0.1173 0.082 Uiso 1 1 calc R . .
C12 C 1.0765(6) 0.2334(4) 0.4328(3) 0.0298(10) Uani 1 1 d . . .
C13 C 1.2452(6) 0.2740(5) 0.5024(4) 0.0379(11) Uani 1 1 d . . .
H13A H 1.2955 0.3637 0.5458 0.046 Uiso 1 1 calc R . .
C14 C 1.2632(7) 0.0419(5) 0.4388(4) 0.0442(12) Uani 1 1 d . . .
H14A H 1.3285 -0.0206 0.4425 0.053 Uiso 1 1 calc R . .
C15 C 1.0969(8) 0.0013(5) 0.3689(4) 0.0420(12) Uani 1 1 d . . .
H15A H 1.0482 -0.0882 0.3252 0.050 Uiso 1 1 calc R . .
C16 C 1.3358(7) 0.1775(6) 0.5052(4) 0.0451(12) Uani 1 1 d . . .
H16A H 1.4482 0.2023 0.5523 0.054 Uiso 1 1 calc R . .
C21 C 0.6527(13) 0.6943(10) 0.1550(8) 0.0295(14) Uani 0.50 1 d PU A 1
H21A H 0.7018 0.7937 0.1878 0.044 Uiso 0.50 1 calc PR A 1
H21B H 0.5271 0.6482 0.1705 0.044 Uiso 0.50 1 calc PR A 1
H21C H 0.6513 0.6897 0.0771 0.044 Uiso 0.50 1 calc PR A 1
C21' C 0.6964(13) 0.7364(10) 0.1960(8) 0.0295(14) Uani 0.50 1 d PU A 2
H21D H 0.6393 0.7431 0.1248 0.044 Uiso 0.50 1 calc PR A 2
H21E H 0.8032 0.8237 0.2213 0.044 Uiso 0.50 1 calc PR A 2
H21F H 0.6070 0.7236 0.2463 0.044 Uiso 0.50 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'
Ni Ni 0.3393 1.1124 '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
N2 Ni1 N2 180.00(12) 2_766 .
N2 Ni1 S3 87.18(11) 2_766 .
N2 Ni1 S3 92.82(11) . .
N2 Ni1 S3 92.82(11) 2_766 2_766
N2 Ni1 S3 87.18(11) . 2_766
S3 Ni1 S3 180.00(6) . 2_766
O1 Ni2 N1 130.40(19) . .
O1 Ni2 S3 117.48(17) . .
N1 Ni2 S3 89.87(12) . .
O1 Ni2 S5 113.73(16) . .
N1 Ni2 S5 96.32(12) . .
S3 Ni2 S5 104.02(6) . .
S2 S3 Ni1 108.72(7) . .
S2 S3 Ni2 100.37(6) . .
Ni1 S3 Ni2 97.82(5) . .
C4 S4 C2 91.1(2) . .
C2 S5 Ni2 97.61(16) . .
C3 S2 S3 102.15(18) . .
C5 S1 C3 89.1(2) . .
C2 N2 C12 113.2(4) . .
C2 N2 Ni1 118.7(3) . .
C12 N2 Ni1 128.0(3) . .
C3 N1 C7 111.0(4) . .
C3 N1 Ni2 122.6(3) . .
C7 N1 Ni2 125.9(3) . .
N2 C2 S5 124.7(3) . .
N2 C2 S4 112.7(3) . .
S5 C2 S4 122.6(3) . .
N1 C3 S2 124.5(4) . .
N1 C3 S1 115.7(4) . .
S2 C3 S1 119.8(3) . .
C15 C4 C12 120.4(4) . .
C15 C4 S4 130.0(4) . .
C12 C4 S4 109.6(3) . .
C7 C5 C9 121.1(5) . .
C7 C5 S1 109.9(4) . .
C9 C5 S1 128.9(4) . .
C21 O1 C21' 30.3(6) . .
C21 O1 Ni2 169.5(6) . .
C21' O1 Ni2 157.9(6) . .
C8 C7 C5 120.1(5) . .
C8 C7 N1 125.6(5) . .
C5 C7 N1 114.3(4) . .
C7 C8 C11 119.2(5) . .
C10 C9 C5 117.8(5) . .
C9 C10 C11 121.3(5) . .
C8 C11 C10 120.4(5) . .
C13 C12 N2 125.6(4) . .
C13 C12 C4 121.0(4) . .
N2 C12 C4 113.4(4) . .
C16 C13 C12 117.8(4) . .
C15 C14 C16 120.6(5) . .
C14 C15 C4 118.3(4) . .
C13 C16 C14 121.9(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 1.908(4) 2_766
Ni1 N2 1.908(4) .
Ni1 S3 2.2452(14) .
Ni1 S3 2.2452(14) 2_766
Ni2 O1 1.657(5) .
Ni2 N1 2.014(4) .
Ni2 S3 2.3356(17) .
Ni2 S5 2.3484(17) .
S3 S2 2.0785(19) .
S4 C4 1.739(5) .
S4 C2 1.756(4) .
S5 C2 1.719(5) .
S2 C3 1.744(5) .
S1 C5 1.748(5) .
S1 C3 1.751(5) .
N2 C2 1.332(6) .
N2 C12 1.408(6) .
N1 C3 1.306(6) .
N1 C7 1.410(6) .
C4 C15 1.401(6) .
C4 C12 1.415(6) .
C5 C7 1.398(7) .
C5 C9 1.409(7) .
O1 C21 1.144(9) .
O1 C21' 1.187(9) .
C7 C8 1.376(7) .
C8 C11 1.380(7) .
C9 C10 1.362(8) .
C10 C11 1.411(9) .
C12 C13 1.385(6) .
C13 C16 1.374(7) .
C14 C15 1.374(7) .
C14 C16 1.410(7) .
