#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179399 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/96/4329689.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_4329689
loop_
_publ_author_name
'Scott R. Daly'
'Jason M. Keith'
'Enrique R. Batista'
'Kevin S. Boland'
'Stosh A. Kozimor'
'Richard L. Martin'
'Brian L. Scott'
_publ_section_title
;
 Probing Ni[S2PR2]2 Electronic Structure to Generate Insight Relevant to
 Minor Actinide Extraction Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7551
_journal_page_last               7560
_journal_paper_doi               10.1021/ic3001587
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C24 H20 Ni P2 S4'
_chemical_formula_weight         557.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.3620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0328(16)
_cell_length_b                   11.4418(14)
_cell_length_c                   16.641(2)
_cell_measurement_temperature    120(1)
_cell_volume                     2414.3(5)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω 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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26270
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.8006
_exptl_absorpt_correction_T_min  0.7297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0397
_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)+(0.0709P)²+0.4362P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                3788
_reflns_number_total             5742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3001587_si_003_3.cif
_cod_data_source_block           apx1135_nis2_ph2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4329689
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Ni1 Ni 0.5000 0.5000 0.0000 0.01346(15) Uani 1 2 d S
S1 S 0.57860(5) 0.32958(6) -0.01240(4) 0.01636(18) Uani 1 1 d .
S2 S 0.48377(6) 0.44303(6) 0.12374(4) 0.01711(18) Uani 1 1 d .
P1 P 0.55770(6) 0.29570(6) 0.10166(4) 0.01423(18) Uani 1 1 d .
C11 C 0.4790(2) 0.1670(2) 0.10294(18) 0.0171(6) Uani 1 1 d .
C12 C 0.3935(2) 0.1485(3) 0.0354(2) 0.0237(7) Uani 1 1 d .
H12 H 0.3819 0.1992 -0.0095 0.028 Uiso 1 1 calc R
C13 C 0.3270(3) 0.0554(3) 0.0357(2) 0.0283(8) Uani 1 1 d .
H13 H 0.2695 0.0443 -0.0086 0.034 Uiso 1 1 calc R
C14 C 0.3451(3) -0.0224(3) 0.1019(2) 0.0304(8) Uani 1 1 d .
H14 H 0.3008 -0.0863 0.1015 0.037 Uiso 1 1 calc R
C15 C 0.4296(3) -0.0038(3) 0.1683(2) 0.0311(8) Uani 1 1 d .
H15 H 0.4417 -0.0554 0.2127 0.037 Uiso 1 1 calc R
C16 C 0.4961(2) 0.0904(3) 0.1693(2) 0.0257(7) Uani 1 1 d .
H16 H 0.5522 0.1025 0.2145 0.031 Uiso 1 1 calc R
C21 C 0.6808(2) 0.2746(2) 0.17667(17) 0.0157(6) Uani 1 1 d .
C22 C 0.7108(2) 0.3502(3) 0.24266(19) 0.0268(7) Uani 1 1 d .
H22 H 0.6659 0.4101 0.2505 0.032 Uiso 1 1 calc R
C23 C 0.8081(3) 0.3366(3) 0.2973(2) 0.0331(8) Uani 1 1 d .
H23 H 0.8284 0.3875 0.3417 0.040 Uiso 1 1 calc R
C24 C 0.8746(2) 0.2480(3) 0.2858(2) 0.0293(8) Uani 1 1 d .
H24 H 0.9395 0.2388 0.3228 0.035 Uiso 1 1 calc R
C25 C 0.8453(2) 0.1723(3) 0.21950(19) 0.0231(7) Uani 1 1 d .
H25 H 0.8907 0.1127 0.2120 0.028 Uiso 1 1 calc R
C26 C 0.7486(2) 0.1853(2) 0.16441(18) 0.0195(6) Uani 1 1 d .
H26 H 0.7290 0.1350 0.1196 0.023 Uiso 1 1 calc R
Ni2 Ni 0.0000 1.0000 0.0000 0.01290(15) Uani 1 2 d S
S3 S -0.02254(6) 0.93608(6) 0.12124(4) 0.01694(18) Uani 1 1 d .
S4 S -0.08752(5) 1.16512(6) 0.01091(4) 0.01531(17) Uani 1 1 d .
P2 P 0.05442(5) 0.79178(6) 0.09797(4) 0.01313(17) Uani 1 1 d .
C31 C 0.1711(2) 0.7613(2) 0.17693(17) 0.0153(6) Uani 1 1 d .
C32 C 0.1808(2) 0.8071(3) 0.25537(18) 0.0215(7) Uani 1 1 d .
H32 H 0.1289 0.8566 0.2660 0.026 Uiso 1 1 calc R
C33 C 0.2678(2) 0.7795(3) 0.31814(19) 0.0287(8) Uani 1 1 d .
H33 H 0.2742 0.8105 0.3707 0.034 Uiso 1 1 calc R
C34 C 0.3443(2) 0.7061(3) 0.3022(2) 0.0267(7) Uani 1 1 d .
H34 H 0.4018 0.6862 0.3444 0.032 Uiso 1 1 calc R
C35 C 0.3362(2) 0.6616(3) 0.22372(19) 0.0227(7) Uani 1 1 d .
H35 H 0.3889 0.6131 0.2132 0.027 Uiso 1 1 calc R
C36 C 0.2500(2) 0.6890(2) 0.16070(18) 0.0185(6) Uani 1 1 d .
H36 H 0.2447 0.6593 0.1079 0.022 Uiso 1 1 calc R
C41 C -0.0273(2) 0.6634(2) 0.09147(17) 0.0175(6) Uani 1 1 d .
C42 C -0.1353(2) 0.6725(3) 0.0602(2) 0.0392(10) Uani 1 1 d .
H42 H -0.1653 0.7453 0.0447 0.047 Uiso 1 1 calc R
C43 C -0.1985(3) 0.5746(3) 0.0519(3) 0.0446(11) Uani 1 1 d .
H43 H -0.2707 0.5819 0.0304 0.053 Uiso 1 1 calc R
C44 C -0.1559(2) 0.4662(3) 0.0750(2) 0.0271(7) Uani 1 1 d .
H44 H -0.1991 0.4007 0.0709 0.033 Uiso 1 1 calc R
C45 C -0.0487(3) 0.4562(3) 0.1042(2) 0.0272(7) Uani 1 1 d .
H45 H -0.0191 0.3830 0.1185 0.033 Uiso 1 1 calc R
C46 C 0.0159(2) 0.5536(3) 0.1125(2) 0.0253(7) Uani 1 1 d .
H46 H 0.0883 0.5455 0.1323 0.030 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'
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
S2 Ni1 S2 179.999(2) . 3_665
S2 Ni1 S1 91.53(3) . 3_665
S2 Ni1 S1 88.47(3) 3_665 3_665
S2 Ni1 S1 88.47(3) . .
S2 Ni1 S1 91.53(3) 3_665 .
S1 Ni1 S1 180.0 3_665 .
P1 S1 Ni1 85.20(3) . .
P1 S2 Ni1 85.66(3) . .
C11 P1 C21 107.48(13) . .
C11 P1 S1 111.72(10) . .
C21 P1 S1 112.61(10) . .
C11 P1 S2 112.63(10) . .
C21 P1 S2 111.77(10) . .
S1 P1 S2 100.66(4) . .
C16 C11 C12 119.6(3) . .
C16 C11 P1 122.7(2) . .
C12 C11 P1 117.6(2) . .
C13 C12 C11 119.9(3) . .
C13 C12 H12 120.0 . .
C11 C12 H12 120.0 . .
C12 C13 C14 120.4(3) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
C15 C14 C13 119.4(3) . .
C15 C14 H14 120.3 . .
C13 C14 H14 120.3 . .
C16 C15 C14 120.7(3) . .
C16 C15 H15 119.6 . .
C14 C15 H15 119.6 . .
C15 C16 C11 119.9(3) . .
C15 C16 H16 120.0 . .
C11 C16 H16 120.0 . .
C22 C21 C26 120.1(3) . .
C22 C21 P1 120.6(2) . .
C26 C21 P1 119.2(2) . .
C21 C22 C23 119.9(3) . .
C21 C22 H22 120.0 . .
C23 C22 H22 120.0 . .
C24 C23 C22 120.1(3) . .
C24 C23 H23 120.0 . .
C22 C23 H23 120.0 . .
C23 C24 C25 120.3(3) . .
C23 C24 H24 119.8 . .
C25 C24 H24 119.8 . .
C24 C25 C26 120.1(3) . .
C24 C25 H25 120.0 . .
C26 C25 H25 120.0 . .
C25 C26 C21 119.5(3) . .
C25 C26 H26 120.3 . .
C21 C26 H26 120.3 . .
S3 Ni2 S3 180.0 3_575 .
S3 Ni2 S4 91.57(3) 3_575 3_575
S3 Ni2 S4 88.43(3) . 3_575
S3 Ni2 S4 88.43(3) 3_575 .
S3 Ni2 S4 91.57(3) . .
S4 Ni2 S4 180.00(3) 3_575 .
P2 S3 Ni2 85.37(3) . .
P2 S4 Ni2 85.11(3) 3_575 .
C31 P2 C41 105.89(13) . .
C31 P2 S3 113.12(10) . .
C41 P2 S3 111.47(10) . .
C31 P2 S4 112.50(10) . 3_575
C41 P2 S4 113.02(10) . 3_575
S3 P2 S4 101.03(4) . 3_575
C32 C31 C36 119.8(3) . .
C32 C31 P2 119.5(2) . .
C36 C31 P2 120.7(2) . .
C31 C32 C33 120.2(3) . .
C31 C32 H32 119.9 . .
C33 C32 H32 119.9 . .
C34 C33 C32 119.7(3) . .
C34 C33 H33 120.1 . .
C32 C33 H33 120.1 . .
C33 C34 C35 120.5(3) . .
C33 C34 H34 119.8 . .
C35 C34 H34 119.8 . .
C34 C35 C36 120.2(3) . .
C34 C35 H35 119.9 . .
C36 C35 H35 119.9 . .
C35 C36 C31 119.6(3) . .
C35 C36 H36 120.2 . .
C31 C36 H36 120.2 . .
C46 C41 C42 118.7(3) . .
C46 C41 P2 121.6(2) . .
C42 C41 P2 119.6(2) . .
C43 C42 C41 120.5(3) . .
C43 C42 H42 119.8 . .
C41 C42 H42 119.8 . .
C44 C43 C42 120.8(3) . .
C44 C43 H43 119.6 . .
C42 C43 H43 119.6 . .
C45 C44 C43 119.0(3) . .
C45 C44 H44 120.5 . .
C43 C44 H44 120.5 . .
C44 C45 C46 120.9(3) . .
C44 C45 H45 119.5 . .
C46 C45 H45 119.5 . .
C45 C46 C41 120.1(3) . .
C45 C46 H46 119.9 . .
C41 C46 H46 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S2 2.2161(7) .
Ni1 S2 2.2161(7) 3_665
Ni1 S1 2.2342(7) 3_665
Ni1 S1 2.2342(7) .
S1 P1 2.0164(10) .
S2 P1 2.0171(10) .
P1 C11 1.797(3) .
P1 C21 1.807(3) .
C11 C16 1.388(4) .
C11 C12 1.404(4) .
C12 C13 1.375(4) .
C12 H12 0.9300 .
C13 C14 1.394(5) .
C13 H13 0.9300 .
C14 C15 1.384(5) .
C14 H14 0.9300 .
C15 C16 1.381(4) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C21 C22 1.381(4) .
C21 C26 1.397(4) .
C22 C23 1.387(4) .
C22 H22 0.9300 .
C23 C24 1.376(4) .
C23 H23 0.9300 .
C24 C25 1.384(4) .
C24 H24 0.9300 .
C25 C26 1.385(4) .
C25 H25 0.9300 .
C26 H26 0.9300 .
Ni2 S3 2.2284(7) 3_575
Ni2 S3 2.2284(7) .
Ni2 S4 2.2358(7) 3_575
Ni2 S4 2.2358(7) .
S3 P2 2.0153(10) .
S4 P2 2.0182(10) 3_575
P2 C31 1.799(3) .
P2 C41 1.803(3) .
P2 S4 2.0182(10) 3_575
C31 C32 1.385(4) .
C31 C36 1.394(4) .
C32 C33 1.388(4) .
C32 H32 0.9300 .
C33 C34 1.376(4) .
C33 H33 0.9300 .
C34 C35 1.382(4) .
C34 H34 0.9300 .
C35 C36 1.385(4) .
C35 H35 0.9300 .
C36 H36 0.9300 .
C41 C46 1.387(4) .
C41 C42 1.388(4) .
C42 C43 1.378(5) .
C42 H42 0.9300 .
C43 C44 1.377(5) .
C43 H43 0.9300 .
C44 C45 1.374(4) .
C44 H44 0.9300 .
C45 C46 1.384(4) .
C45 H45 0.9300 .
C46 H46 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C12 C11 P1 S1 -38.8(2)
C12 C11 P1 S2 73.6(2)
C22 C21 P1 S1 116.7(2)
C22 C21 P1 S2 4.3(3)
