#------------------------------------------------------------------------------
#$Date: 2020-11-05 10:56:28 +0200 (Thu, 05 Nov 2020) $
#$Revision: 258736 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/69/4306994.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_4306994
loop_
_publ_author_name
'Stephen P. Jeffery'
'Michael L. Singleton'
'Joseph H. Reibenspies'
'Marcetta Y. Darensbourg'
_publ_contact_author_address
;Texas A&M University
Department of Chemistry
College Station, TX 77843-3255
USA            
;
_publ_contact_author_email       marcetta@mail.chem.tamu.edu
_publ_contact_author_fax         979-845-0158
_publ_contact_author_name        'Marcetta Y. Darensbourg'
_publ_contact_author_phone       959-845-5417
_publ_section_title
;
Control of S-Based Aggregation: Designed Synthesis of NiM2 and Ni2M
Trinuclear Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              179
_journal_page_last               185
_journal_paper_doi               10.1021/ic061475f
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C20 H20 N2 Ni O10 S2 W2'
_chemical_formula_weight         938.91
_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                106.304(5)
_cell_angle_beta                 96.606(4)
_cell_angle_gamma                112.242(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4829(7)
_cell_length_b                   10.5887(7)
_cell_length_c                   13.7992(8)
_cell_measurement_reflns_used    1950
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      57.38
_cell_measurement_theta_min      4.71
_cell_volume                     1317.83(16)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11485
_diffrn_reflns_theta_full        58.93
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    18.591
_exptl_absorpt_correction_T_max  0.8359
_exptl_absorpt_correction_T_min  0.0946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.366
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.00020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [0.00000+1.00000exp(1.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0000P)²+0.0000sinθ/λ] 
 where P = 0.33333Fo² + 0.66667Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                2842
_reflns_number_total             3652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061475fsi20060804_042402_2.cif
_cod_data_source_block           md307a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

2020-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H40 N4 Ni2 O20 S4 W4'
_cod_original_formula_weight         1877.82
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1317.83(15)
_cod_database_code               4306994
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
W1A W 0.88532(4) 1.00205(4) 0.21791(3) 0.01723(18) Uani 1 1 d . . .
W2A W 0.62302(4) 0.51574(4) 0.32971(3) 0.01636(18) Uani 1 1 d . . .
Ni1A Ni 0.48036(15) 0.76415(15) 0.22696(12) 0.0136(4) Uani 1 1 d . . .
S1A S 0.6976(2) 0.9147(2) 0.31832(18) 0.0167(5) Uani 1 1 d . . .
S2A S 0.5497(2) 0.5924(2) 0.17925(18) 0.0157(5) Uani 1 1 d . . .
O1A O 0.6442(8) 0.9193(8) 0.0208(6) 0.0312(18) Uani 1 1 d . . .
O2A O 0.9426(9) 1.3373(9) 0.3009(7) 0.043(2) Uani 1 1 d . . .
O3A O 1.1231(8) 1.1048(9) 0.1026(6) 0.038(2) Uani 1 1 d . . .
O4A O 1.1137(8) 1.0748(8) 0.4234(6) 0.0315(18) Uani 1 1 d . . .
O5A O 0.8836(7) 0.6904(8) 0.1267(6) 0.0305(19) Uani 1 1 d . . .
O6A O 0.9472(8) 0.7401(8) 0.3771(6) 0.0347(19) Uani 1 1 d . . .
O7A O 0.6676(8) 0.2868(8) 0.1478(6) 0.0298(18) Uani 1 1 d . . .
O8A O 0.7463(8) 0.4344(8) 0.5089(6) 0.0337(19) Uani 1 1 d . . .
O9A O 0.3179(8) 0.2800(8) 0.3183(6) 0.0341(19) Uani 1 1 d . . .
O10A O 0.5557(7) 0.7516(7) 0.4881(5) 0.0228(16) Uani 1 1 d . . .
N1A N 0.4258(8) 0.9283(8) 0.2489(6) 0.0164(18) Uani 1 1 d . . .
N2A N 0.2784(8) 0.6207(8) 0.1658(6) 0.0161(18) Uani 1 1 d . . .
C1A C 0.7324(11) 0.9503(11) 0.0923(8) 0.023(2) Uani 1 1 d U . .
C2A C 0.9155(11) 1.2180(13) 0.2738(9) 0.027(3) Uani 1 1 d . . .
C3A C 1.0369(11) 1.0681(10) 0.1455(8) 0.022(2) Uani 1 1 d . . .
C4A C 1.0307(11) 1.0488(10) 0.3509(9) 0.024(2) Uani 1 1 d . . .
C5A C 0.8803(10) 0.7970(11) 0.1590(8) 0.022(2) Uani 1 1 d U . .
C6A C 0.8286(12) 0.6633(11) 0.3577(8) 0.024(2) Uani 1 1 d . . .
C7A C 0.6545(11) 0.3681(13) 0.2162(10) 0.033(3) Uani 1 1 d . . .
C8A C 0.6970(11) 0.4619(11) 0.4418(9) 0.029(3) Uani 1 1 d . . .
C9A C 0.4263(11) 0.3633(11) 0.3187(7) 0.018(2) Uani 1 1 d U . .
C10A C 0.5833(10) 0.6699(11) 0.4333(8) 0.019(2) Uani 1 1 d U . .
C11A C 0.6508(10) 1.0611(10) 0.3787(8) 0.021(2) Uani 1 1 d U . .
H11A H 0.6057 1.0425 0.4356 0.025 Uiso 1 1 calc R . .
H11B H 0.7373 1.1549 0.4087 0.025 Uiso 1 1 calc R . .
C12A C 0.5509(10) 1.0683(10) 0.2982(8) 0.0192(19) Uani 1 1 d U . .
H12A H 0.5206 1.1448 0.3305 0.023 Uiso 1 1 calc R . .
H12B H 0.5994 1.0949 0.2447 0.023 Uiso 1 1 calc R . .
C13A C 0.3211(10) 0.9182(11) 0.3151(8) 0.022(2) Uani 1 1 d U . .
H13A H 0.2412 0.9316 0.2811 0.026 Uiso 1 1 calc R . .
H13B H 0.3682 0.9987 0.3833 0.026 Uiso 1 1 calc R . .
C14A C 0.2623(10) 0.7760(10) 0.3336(8) 0.0208(18) Uani 1 1 d U . .
H14A H 0.3419 0.7661 0.3717 0.025 Uiso 1 1 calc R . .
H14B H 0.1964 0.7796 0.3791 0.025 Uiso 1 1 calc R . .
C15A C 0.1851(10) 0.6430(11) 0.2376(8) 0.020(2) Uani 1 1 d U . .
H15A H 0.1043 0.6513 0.1995 0.024 Uiso 1 1 calc R . .
H15B H 0.1456 0.5565 0.2583 0.024 Uiso 1 1 calc R . .
C16A C 0.3631(11) 0.9192(11) 0.1427(8) 0.023(2) Uani 1 1 d U . .
H16A H 0.4346 0.9232 0.1012 0.028 Uiso 1 1 calc R . .
H16B H 0.3453 1.0064 0.1501 0.028 Uiso 1 1 calc R . .
C17A C 0.2260(10) 0.7850(11) 0.0817(8) 0.0236(19) Uani 1 1 d U . .
H17A H 0.1506 0.7879 0.1183 0.028 Uiso 1 1 calc R . .
H17B H 0.1974 0.7895 0.0123 0.028 Uiso 1 1 calc R . .
C18A C 0.2328(11) 0.6407(11) 0.0664(8) 0.023(2) Uani 1 1 d U . .
H18A H 0.1376 0.5608 0.0278 0.028 Uiso 1 1 calc R . .
H18B H 0.2999 0.6323 0.0228 0.028 Uiso 1 1 calc R . .
C19A C 0.2624(10) 0.4667(10) 0.1393(8) 0.021(2) Uani 1 1 d U . .
H19A H 0.2626 0.4414 0.2031 0.025 Uiso 1 1 calc R . .
H19B H 0.1698 0.3992 0.0886 0.025 Uiso 1 1 calc R . .
C20A C 0.3795(10) 0.4476(10) 0.0940(8) 0.019(2) Uani 1 1 d U . .
H20A H 0.3685 0.4530 0.0233 0.023 Uiso 1 1 calc R . .
H20B H 0.3760 0.3510 0.0886 0.023 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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
C3A W1A C1A 91.8(4) . . ?
C3A W1A C4A 92.1(4) . . ?
C1A W1A C4A 176.1(4) . . ?
C3A W1A C5A 86.9(4) . . ?
C1A W1A C5A 89.8(4) . . ?
C4A W1A C5A 90.0(4) . . ?
C3A W1A C2A 86.4(4) . . ?
C1A W1A C2A 92.8(4) . . ?
C4A W1A C2A 87.8(4) . . ?
C5A W1A C2A 172.9(4) . . ?
C3A W1A S1A 177.1(3) . . ?
C1A W1A S1A 90.9(3) . . ?
C4A W1A S1A 85.2(3) . . ?
C5A W1A S1A 92.1(3) . . ?
C2A W1A S1A 94.5(3) . . ?
C8A W2A C7A 93.4(4) . . ?
C8A W2A C9A 87.6(4) . . ?
C7A W2A C9A 91.1(4) . . ?
C8A W2A C6A 85.0(4) . . ?
C7A W2A C6A 90.4(4) . . ?
C9A W2A C6A 172.5(4) . . ?
C8A W2A C10A 92.1(4) . . ?
C7A W2A C10A 174.5(4) . . ?
C9A W2A C10A 89.0(4) . . ?
C6A W2A C10A 90.3(4) . . ?
C8A W2A S2A 174.5(3) . . ?
C7A W2A S2A 83.8(3) . . ?
C9A W2A S2A 97.2(3) . . ?
C6A W2A S2A 90.3(3) . . ?
C10A W2A S2A 90.7(3) . . ?
N2A Ni1A N1A 90.9(3) . . ?
N2A Ni1A S2A 90.8(2) . . ?
N1A Ni1A S2A 170.1(3) . . ?
N2A Ni1A S1A 170.4(3) . . ?
N1A Ni1A S1A 90.7(2) . . ?
S2A Ni1A S1A 89.25(9) . . ?
C11A S1A Ni1A 94.2(3) . . ?
C11A S1A W1A 109.4(4) . . ?
Ni1A S1A W1A 117.47(11) . . ?
C20A S2A Ni1A 97.8(3) . . ?
C20A S2A W2A 108.8(4) . . ?
Ni1A S2A W2A 113.39(10) . . ?
C12A N1A C16A 108.3(8) . . ?
C12A N1A C13A 109.1(7) . . ?
C16A N1A C13A 111.2(7) . . ?
C12A N1A Ni1A 110.8(5) . . ?
C16A N1A Ni1A 106.2(5) . . ?
C13A N1A Ni1A 111.2(6) . . ?
C18A N2A C15A 110.5(7) . . ?
C18A N2A C19A 108.0(7) . . ?
C15A N2A C19A 108.4(8) . . ?
C18A N2A Ni1A 106.2(6) . . ?
C15A N2A Ni1A 112.2(5) . . ?
C19A N2A Ni1A 111.4(5) . . ?
O1A C1A W1A 179.2(10) . . ?
O2A C2A W1A 173.8(10) . . ?
O3A C3A W1A 179.1(9) . . ?
O4A C4A W1A 178.4(9) . . ?
O5A C5A W1A 176.8(9) . . ?
O6A C6A W2A 174.8(9) . . ?
O7A C7A W2A 175.8(9) . . ?
O8A C8A W2A 177.2(10) . . ?
O9A C9A W2A 176.2(8) . . ?
O10A C10A W2A 177.2(8) . . ?
C12A C11A S1A 108.3(7) . . ?
N1A C12A C11A 111.0(8) . . ?
N1A C13A C14A 113.9(8) . . ?
C15A C14A C13A 115.3(9) . . ?
C14A C15A N2A 113.0(8) . . ?
N1A C16A C17A 116.0(9) . . ?
C18A C17A C16A 115.4(8) . . ?
N2A C18A C17A 114.1(8) . . ?
C20A C19A N2A 111.7(8) . . ?
C19A C20A S2A 108.5(6) . . ?
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
W1A C3A 1.982(12) . ?
W1A C1A 2.010(11) . ?
W1A C4A 2.053(12) . ?
W1A C5A 2.071(11) . ?
W1A C2A 2.081(12) . ?
W1A S1A 2.572(3) . ?
W2A C8A 1.968(13) . ?
W2A C7A 2.035(13) . ?
W2A C9A 2.037(12) . ?
W2A C6A 2.038(12) . ?
W2A C10A 2.055(11) . ?
W2A S2A 2.571(2) . ?
Ni1A N2A 1.984(8) . ?
Ni1A N1A 1.984(7) . ?
Ni1A S2A 2.170(2) . ?
Ni1A S1A 2.186(3) . ?
S1A C11A 1.813(9) . ?
S2A C20A 1.831(9) . ?
O1A C1A 1.146(12) . ?
O2A C2A 1.120(13) . ?
O3A C3A 1.142(13) . ?
O4A C4A 1.138(13) . ?
O5A C5A 1.107(11) . ?
O6A C6A 1.147(13) . ?
O7A C7A 1.147(14) . ?
O8A C8A 1.168(14) . ?
O9A C9A 1.144(13) . ?
O10A C10A 1.130(12) . ?
N1A C12A 1.461(13) . ?
N1A C16A 1.497(13) . ?
N1A C13A 1.499(13) . ?
N2A C18A 1.497(13) . ?
N2A C15A 1.504(12) . ?
N2A C19A 1.505(12) . ?
C11A C12A 1.475(14) . ?
C13A C14A 1.503(15) . ?
C14A C15A 1.495(14) . ?
C16A C17A 1.516(14) . ?
C17A C18A 1.513(14) . ?
C19A C20A 1.494(14) . ?
