#------------------------------------------------------------------------------
#$Date: 2017-03-02 19:20:33 +0200 (Thu, 02 Mar 2017) $
#$Revision: 192782 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/59/4305961.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_4305961
loop_
_publ_author_name
'Kuppuswamy Arumugam'
'Rongmin Yu'
'Dino Villagrán'
'Thomas G. Gray'
'Joel T. Mague'
'James P. Donahue'
_publ_contact_author_email       donahue@tulane.edu
_publ_contact_author_fax         504-865-5596
_publ_contact_author_phone       504-862-3562
_publ_section_title
;
A Convergent Approach to the Synthesis of Multimetallic Dithiolene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5570
_journal_page_last               5572
_journal_paper_doi               10.1021/ic800880s
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C33 H50 Ni O P2 S4'
_chemical_formula_weight         711.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 102.639(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0645(19)
_cell_length_b                   17.391(3)
_cell_length_c                   16.307(3)
_cell_measurement_reflns_used    6599
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2645
_cell_measurement_theta_min      2.2455
_cell_volume                     3338.5(10)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX'
_diffrn_measurement_method       'phi and 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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30314
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.9476
_exptl_absorpt_correction_T_min  0.7694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plates
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         8015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0460
_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)+(0.0567P)²+2.8363P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                6599
_reflns_number_total             8015
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic800880s-file004_2.cif
_cod_data_source_block           '[(dcpe)Ni(S2C6H2S2CO)]'
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_publ-contact_author-phone' replaced with
'_publ_contact_author_phone' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        3338.6(9)
_cod_database_code               4305961
loop_
_publ_contact_author_name
_publ_contact_author_address
'Dr. James P. Donahue'
;
  Department of Chemistry
  Tulane University
  6400 Freret Street
  New Orleans, LA 70118-5698
  Unites States of America
;
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.67056(3) 0.205164(18) 0.261992(19) 0.01341(9) Uani 1 1 d . . .
S1 S 0.58434(5) 0.15684(4) 0.35359(4) 0.01931(15) Uani 1 1 d . . .
S2 S 0.82181(5) 0.13715(4) 0.31069(4) 0.01919(15) Uani 1 1 d . . .
S3 S 0.67562(5) -0.09339(4) 0.56574(4) 0.01884(14) Uani 1 1 d . . .
S4 S 0.89483(6) -0.11849(4) 0.51580(5) 0.02775(17) Uani 1 1 d . . .
P1 P 0.52139(5) 0.27653(4) 0.20975(4) 0.01393(14) Uani 1 1 d . . .
P2 P 0.75523(5) 0.25829(4) 0.17081(4) 0.01410(14) Uani 1 1 d . . .
O1 O 0.81338(19) -0.20975(12) 0.61725(14) 0.0319(5) Uani 1 1 d . . .
C1 C 0.6743(2) 0.08339(14) 0.40269(15) 0.0144(5) Uani 1 1 d . . .
C2 C 0.7820(2) 0.07481(14) 0.38330(15) 0.0162(5) Uani 1 1 d . . .
C3 C 0.7113(2) -0.02668(14) 0.49483(15) 0.0149(5) Uani 1 1 d . . .
C4 C 0.8164(2) -0.03706(15) 0.47343(16) 0.0183(5) Uani 1 1 d . . .
C5 C 0.6409(2) 0.03342(14) 0.45969(15) 0.0161(5) Uani 1 1 d . . .
H5 H 0.5697 0.0405 0.4745 0.019 Uiso 1 1 calc R . .
C6 C 0.8524(2) 0.01460(15) 0.41961(17) 0.0209(6) Uani 1 1 d . . .
H6 H 0.9255 0.0089 0.4075 0.025 Uiso 1 1 calc R . .
C7 C 0.7980(2) -0.15260(16) 0.57514(17) 0.0228(6) Uani 1 1 d . . .
C8 C 0.3854(2) 0.23177(15) 0.15583(15) 0.0163(5) Uani 1 1 d . . .
H8 H 0.3340 0.2746 0.1302 0.020 Uiso 1 1 calc R . .
C9 C 0.3998(2) 0.17893(16) 0.08352(17) 0.0222(6) Uani 1 1 d . . .
H9A H 0.4301 0.2092 0.0419 0.027 Uiso 1 1 calc R . .
H9B H 0.4556 0.1381 0.1057 0.027 Uiso 1 1 calc R . .
C10 C 0.2872(2) 0.14185(17) 0.04010(18) 0.0266(6) Uani 1 1 d . . .
H10A H 0.2359 0.1820 0.0099 0.032 Uiso 1 1 calc R . .
H10B H 0.3015 0.1042 -0.0019 0.032 Uiso 1 1 calc R . .
C11 C 0.2290(2) 0.10125(16) 0.10214(19) 0.0258(6) Uani 1 1 d . . .
H11A H 0.1544 0.0812 0.0720 0.031 Uiso 1 1 calc R . .
H11B H 0.2760 0.0572 0.1278 0.031 Uiso 1 1 calc R . .
C12 C 0.2122(2) 0.15651(17) 0.17072(18) 0.0256(6) Uani 1 1 d . . .
H12A H 0.1761 0.1290 0.2112 0.031 Uiso 1 1 calc R . .
H12B H 0.1610 0.1988 0.1454 0.031 Uiso 1 1 calc R . .
C13 C 0.3258(2) 0.18987(17) 0.21681(17) 0.0233(6) Uani 1 1 d . . .
H13A H 0.3752 0.1479 0.2450 0.028 Uiso 1 1 calc R . .
H13B H 0.3130 0.2262 0.2605 0.028 Uiso 1 1 calc R . .
C14 C 0.4770(2) 0.34192(14) 0.28543(16) 0.0167(5) Uani 1 1 d . . .
H14 H 0.4439 0.3092 0.3245 0.020 Uiso 1 1 calc R . .
C15 C 0.5793(2) 0.38349(16) 0.33888(17) 0.0204(5) Uani 1 1 d . . .
H15A H 0.6168 0.4147 0.3020 0.024 Uiso 1 1 calc R . .
H15B H 0.6349 0.3451 0.3680 0.024 Uiso 1 1 calc R . .
C16 C 0.5435(2) 0.43581(15) 0.40402(17) 0.0210(6) Uani 1 1 d . . .
H16A H 0.5142 0.4040 0.4449 0.025 Uiso 1 1 calc R . .
H16B H 0.6105 0.4646 0.4351 0.025 Uiso 1 1 calc R . .
C17 C 0.4523(2) 0.49226(16) 0.36198(18) 0.0246(6) Uani 1 1 d . . .
H17A H 0.4282 0.5237 0.4056 0.029 Uiso 1 1 calc R . .
H17B H 0.4843 0.5274 0.3253 0.029 Uiso 1 1 calc R . .
C18 C 0.3502(2) 0.45142(16) 0.31014(18) 0.0244(6) Uani 1 1 d . . .
H18A H 0.2944 0.4899 0.2817 0.029 Uiso 1 1 calc R . .
H18B H 0.3136 0.4203 0.3476 0.029 Uiso 1 1 calc R . .
C19 C 0.3839(2) 0.39891(15) 0.24397(16) 0.0195(5) Uani 1 1 d . . .
H19A H 0.4119 0.4306 0.2023 0.023 Uiso 1 1 calc R . .
H19B H 0.3164 0.3701 0.2139 0.023 Uiso 1 1 calc R . .
C20 C 0.8355(2) 0.19639(14) 0.11275(16) 0.0169(5) Uani 1 1 d . . .
H20 H 0.9094 0.1841 0.1520 0.020 Uiso 1 1 calc R . .
C21 C 0.7746(2) 0.11968(15) 0.08786(17) 0.0215(6) Uani 1 1 d . . .
H21A H 0.7029 0.1288 0.0461 0.026 Uiso 1 1 calc R . .
H21B H 0.7559 0.0952 0.1379 0.026 Uiso 1 1 calc R . .
C22 C 0.8522(3) 0.06655(16) 0.05033(19) 0.0266(6) Uani 1 1 d . . .
H22A H 0.9222 0.0557 0.0934 0.032 Uiso 1 1 calc R . .
H22B H 0.8129 0.0171 0.0341 0.032 Uiso 1 1 calc R . .
C23 C 0.8843(3) 0.10278(18) -0.02661(18) 0.0279(6) Uani 1 1 d . . .
H23A H 0.8155 0.1072 -0.0724 0.034 Uiso 1 1 calc R . .
H23B H 0.9390 0.0690 -0.0465 0.034 Uiso 1 1 calc R . .
C24 C 0.9370(2) 0.18245(17) -0.00649(18) 0.0260(6) Uani 1 1 d . . .
H24A H 1.0128 0.1767 0.0314 0.031 Uiso 1 1 calc R . .
H24B H 0.9477 0.2067 -0.0591 0.031 Uiso 1 1 calc R . .
C25 C 0.8640(2) 0.23501(16) 0.03508(17) 0.0220(6) Uani 1 1 d . . .
H25A H 0.7927 0.2475 -0.0058 0.026 Uiso 1 1 calc R . .
H25B H 0.9052 0.2837 0.0520 0.026 Uiso 1 1 calc R . .
C26 C 0.8525(2) 0.33638(15) 0.22041(19) 0.0252(6) Uani 1 1 d . . .
H26 H 0.8252 0.3513 0.2719 0.030 Uiso 1 1 calc R . .
C27 C 0.9746(2) 0.30657(15) 0.25297(17) 0.0197(5) Uani 1 1 d . . .
H27A H 0.9731 0.2619 0.2904 0.024 Uiso 1 1 calc R . .
H27B H 1.0058 0.2890 0.2048 0.024 Uiso 1 1 calc R . .
C28 C 1.0519(3) 0.36880(18) 0.3011(2) 0.0324(7) Uani 1 1 d . . .
H28A H 1.0282 0.3800 0.3543 0.039 Uiso 1 1 calc R . .
H28B H 1.1310 0.3494 0.3155 0.039 Uiso 1 1 calc R . .
C29 C 1.0482(3) 0.44108(17) 0.2517(2) 0.0340(7) Uani 1 1 d . . .
H29A H 1.0820 0.4315 0.2025 0.041 Uiso 1 1 calc R . .
H29B H 1.0946 0.4808 0.2869 0.041 Uiso 1 1 calc R . .
C30 C 0.9270(2) 0.47116(16) 0.2213(2) 0.0279(6) Uani 1 1 d . . .
H30A H 0.9282 0.5174 0.1861 0.034 Uiso 1 1 calc R . .
H30B H 0.8961 0.4862 0.2704 0.034 Uiso 1 1 calc R . .
C31 C 0.8500(3) 0.41006(17) 0.1702(2) 0.0310(7) Uani 1 1 d . . .
H31A H 0.7712 0.4297 0.1547 0.037 Uiso 1 1 calc R . .
H31B H 0.8757 0.3993 0.1177 0.037 Uiso 1 1 calc R . .
C32 C 0.5561(2) 0.34027(15) 0.12863(16) 0.0183(5) Uani 1 1 d . . .
H32A H 0.4867 0.3506 0.0849 0.022 Uiso 1 1 calc R . .
H32B H 0.5852 0.3899 0.1543 0.022 Uiso 1 1 calc R . .
C33 C 0.6459(2) 0.30262(15) 0.08857(16) 0.0177(5) Uani 1 1 d . . .
H33A H 0.6808 0.3418 0.0581 0.021 Uiso 1 1 calc R . .
H33B H 0.6099 0.2630 0.0477 0.021 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
S1 Ni1 S2 91.62(3) . . ?
S1 Ni1 P2 177.77(3) . . ?
S2 Ni1 P2 89.92(3) . . ?
S1 Ni1 P1 90.59(3) . . ?
S2 Ni1 P1 177.75(3) . . ?
P2 Ni1 P1 87.85(3) . . ?
C1 S1 Ni1 104.75(9) . . ?
C2 S2 Ni1 104.60(9) . . ?
C3 S3 C7 96.93(12) . . ?
C4 S4 C7 97.01(13) . . ?
C14 P1 C32 104.75(12) . . ?
C14 P1 C8 102.71(11) . . ?
C32 P1 C8 103.23(12) . . ?
C14 P1 Ni1 114.97(8) . . ?
C32 P1 Ni1 108.79(8) . . ?
C8 P1 Ni1 120.73(9) . . ?
C33 P2 C20 104.17(12) . . ?
C33 P2 C26 107.19(12) . . ?
C20 P2 C26 107.32(13) . . ?
C33 P2 Ni1 107.88(8) . . ?
C20 P2 Ni1 118.64(8) . . ?
C26 P2 Ni1 110.92(10) . . ?
C5 C1 C2 119.9(2) . . ?
C5 C1 S1 121.20(18) . . ?
C2 C1 S1 118.92(19) . . ?
C6 C2 C1 119.3(2) . . ?
C6 C2 S2 121.39(19) . . ?
C1 C2 S2 119.27(19) . . ?
C5 C3 C4 120.0(2) . . ?
C5 C3 S3 123.58(19) . . ?
C4 C3 S3 116.42(19) . . ?
C6 C4 C3 120.0(2) . . ?
C6 C4 S4 123.6(2) . . ?
C3 C4 S4 116.43(19) . . ?
C3 C5 C1 120.3(2) . . ?
C4 C6 C2 120.5(2) . . ?
O1 C7 S4 123.5(2) . . ?
O1 C7 S3 123.4(2) . . ?
S4 C7 S3 113.11(15) . . ?
C13 C8 C9 111.2(2) . . ?
C13 C8 P1 112.56(17) . . ?
C9 C8 P1 112.22(17) . . ?
C10 C9 C8 111.7(2) . . ?
C11 C10 C9 112.3(2) . . ?
C12 C11 C10 110.5(2) . . ?
C11 C12 C13 110.6(2) . . ?
C12 C13 C8 111.1(2) . . ?
C15 C14 C19 111.5(2) . . ?
C15 C14 P1 110.94(17) . . ?
C19 C14 P1 113.24(17) . . ?
C14 C15 C16 111.2(2) . . ?
C17 C16 C15 110.9(2) . . ?
C18 C17 C16 111.7(2) . . ?
C17 C18 C19 111.4(2) . . ?
C18 C19 C14 110.8(2) . . ?
C21 C20 C25 110.0(2) . . ?
C21 C20 P2 111.66(17) . . ?
C25 C20 P2 113.92(18) . . ?
C20 C21 C22 109.3(2) . . ?
C23 C22 C21 111.4(2) . . ?
C22 C23 C24 111.4(2) . . ?
C25 C24 C23 112.6(2) . . ?
C24 C25 C20 111.0(2) . . ?
C31 C26 C27 112.0(2) . . ?
C31 C26 P2 116.5(2) . . ?
C27 C26 P2 111.61(18) . . ?
C28 C27 C26 111.6(2) . . ?
C29 C28 C27 112.1(3) . . ?
C28 C29 C30 112.2(3) . . ?
C29 C30 C31 111.2(2) . . ?
C26 C31 C30 110.7(2) . . ?
C33 C32 P1 110.03(17) . . ?
C32 C33 P2 109.34(17) . . ?
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
Ni1 S1 2.1678(7) . ?
Ni1 S2 2.1738(7) . ?
Ni1 P2 2.1847(7) . ?
Ni1 P1 2.1987(7) . ?
S1 C1 1.753(2) . ?
S2 C2 1.748(3) . ?
S3 C3 1.757(2) . ?
S3 C7 1.780(3) . ?
S4 C4 1.758(3) . ?
S4 C7 1.774(3) . ?
P1 C14 1.842(3) . ?
P1 C32 1.843(3) . ?
P1 C8 1.855(3) . ?
P2 C33 1.833(3) . ?
P2 C20 1.842(3) . ?
P2 C26 1.860(3) . ?
O1 C7 1.199(3) . ?
C1 C5 1.395(3) . ?
C1 C2 1.411(3) . ?
C2 C6 1.396(4) . ?
C3 C5 1.389(3) . ?
C3 C4 1.399(3) . ?
C4 C6 1.390(4) . ?
C8 C13 1.532(4) . ?
C8 C9 1.535(3) . ?
C9 C10 1.530(4) . ?
C10 C11 1.525(4) . ?
C11 C12 1.521(4) . ?
C12 C13 1.526(4) . ?
C14 C15 1.528(3) . ?
C14 C19 1.539(3) . ?
C15 C16 1.531(4) . ?
C16 C17 1.522(4) . ?
C17 C18 1.510(4) . ?
C18 C19 1.535(4) . ?
C20 C21 1.534(3) . ?
C20 C25 1.538(3) . ?
C21 C22 1.535(4) . ?
C22 C23 1.527(4) . ?
C23 C24 1.530(4) . ?
C24 C25 1.527(4) . ?
C26 C31 1.518(4) . ?
C26 C27 1.543(4) . ?
C27 C28 1.529(4) . ?
C28 C29 1.489(4) . ?
C29 C30 1.530(4) . ?
C30 C31 1.532(4) . ?
C32 C33 1.529(3) . ?
