#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179399 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/96/4329688.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_4329688
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            'C28 H16 F12 Ni P2 S4'
_chemical_formula_weight         829.30
_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                 92.802(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.803(6)
_cell_length_b                   11.195(6)
_cell_length_c                   13.291(7)
_cell_measurement_temperature    120(1)
_cell_volume                     1605.5(15)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15525
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.8839
_exptl_absorpt_correction_T_min  0.6314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3065
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.336
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0416
_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)+(0.0330P)²+1.5780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                2520
_reflns_number_total             3065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3001587_si_003_2.cif
_cod_data_source_block           apx1420
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329688
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 1.0000 1.0000 0.0000 0.02048(19) Uani 1 2 d S . .
S1 S 0.87752(9) 1.03967(8) 0.12631(7) 0.0242(2) Uani 1 1 d . . .
S2 S 1.03511(9) 0.81867(8) 0.06648(7) 0.0241(2) Uani 1 1 d . . .
P1 P 0.95160(9) 0.88919(8) 0.18502(7) 0.0210(2) Uani 1 1 d . . .
C11 C 1.0641(3) 0.9147(3) 0.2879(3) 0.0213(8) Uani 1 1 d . . .
C12 C 1.0482(4) 1.0096(3) 0.3538(3) 0.0252(8) Uani 1 1 d . . .
H12 H 0.9817 1.0616 0.3430 0.030 Uiso 1 1 calc R . .
C13 C 1.1310(4) 1.0266(3) 0.4350(3) 0.0270(9) Uani 1 1 d . . .
H13 H 1.1212 1.0909 0.4783 0.032 Uiso 1 1 calc R . .
C14 C 1.2289(3) 0.9473(3) 0.4519(3) 0.0258(8) Uani 1 1 d . . .
C15 C 1.2462(4) 0.8541(4) 0.3861(3) 0.0300(9) Uani 1 1 d . . .
H15 H 1.3123 0.8019 0.3974 0.036 Uiso 1 1 calc R . .
C16 C 1.1647(3) 0.8383(3) 0.3031(3) 0.0273(9) Uani 1 1 d . . .
H16 H 1.1774 0.7767 0.2578 0.033 Uiso 1 1 calc R . .
C17 C 1.3127(4) 0.9632(4) 0.5436(3) 0.0357(10) Uani 1 1 d . . .
F11 F 1.4135(3) 0.8965(3) 0.5435(2) 0.0578(8) Uani 1 1 d . . .
F12 F 1.3519(3) 1.0765(3) 0.5548(2) 0.0601(8) Uani 1 1 d . . .
F13 F 1.2557(2) 0.9385(3) 0.62799(19) 0.0620(9) Uani 1 1 d . . .
C21 C 0.8331(3) 0.7947(3) 0.2334(3) 0.0209(8) Uani 1 1 d . . .
C22 C 0.7211(4) 0.7841(4) 0.1785(3) 0.0353(10) Uani 1 1 d . . .
H22 H 0.7069 0.8279 0.1196 0.042 Uiso 1 1 calc R . .
C23 C 0.6308(4) 0.7080(4) 0.2115(3) 0.0409(11) Uani 1 1 d . . .
H23 H 0.5558 0.7006 0.1746 0.049 Uiso 1 1 calc R . .
C24 C 0.6515(4) 0.6433(4) 0.2990(3) 0.0347(10) Uani 1 1 d . A .
C25 C 0.7618(4) 0.6539(4) 0.3545(3) 0.0318(9) Uani 1 1 d . . .
H25 H 0.7755 0.6102 0.4135 0.038 Uiso 1 1 calc R . .
C26 C 0.8527(4) 0.7306(3) 0.3217(3) 0.0259(8) Uani 1 1 d . . .
H26 H 0.9271 0.7389 0.3594 0.031 Uiso 1 1 calc R . .
C27 C 0.5533(4) 0.5610(4) 0.3334(3) 0.0566(14) Uani 1 1 d D . .
F21A F 0.5244(6) 0.4774(5) 0.2596(5) 0.070(2) Uani 0.554(10) 1 d PDU A 1
F22A F 0.5847(9) 0.4961(8) 0.4113(6) 0.087(3) Uani 0.554(10) 1 d PDU A 1
F23A F 0.4464(5) 0.6118(5) 0.3415(8) 0.083(3) Uani 0.554(10) 1 d PDU A 1
F21B F 0.4547(8) 0.5474(12) 0.2765(8) 0.115(5) Uani 0.446(10) 1 d PDU A 2
F22B F 0.5085(10) 0.6098(7) 0.4191(7) 0.090(4) Uani 0.446(10) 1 d PDU A 2
F23B F 0.5937(10) 0.4579(6) 0.3671(8) 0.073(3) Uani 0.446(10) 1 d PDU 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'
F F 0.0171 0.0103 '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
S1 Ni1 S1 180.0 . 3_775
S1 Ni1 S2 88.79(4) . .
S1 Ni1 S2 91.21(4) 3_775 .
S1 Ni1 S2 91.21(4) . 3_775
S1 Ni1 S2 88.78(4) 3_775 3_775
S2 Ni1 S2 180.0 . 3_775
S1 Ni1 P1 135.14(4) . 3_775
S1 Ni1 P1 44.86(4) 3_775 3_775
S2 Ni1 P1 134.95(3) . 3_775
S2 Ni1 P1 45.05(3) 3_775 3_775
S1 Ni1 P1 44.86(4) . .
S1 Ni1 P1 135.14(4) 3_775 .
S2 Ni1 P1 45.05(3) . .
S2 Ni1 P1 134.95(3) 3_775 .
P1 Ni1 P1 179.999(1) 3_775 .
P1 S1 Ni1 83.43(5) . .
P1 S2 Ni1 83.09(5) . .
C21 P1 C11 106.60(16) . .
C21 P1 S1 110.78(13) . .
C11 P1 S1 113.71(13) . .
C21 P1 S2 113.67(12) . .
C11 P1 S2 110.10(13) . .
S1 P1 S2 102.13(6) . .
C21 P1 Ni1 137.10(12) . .
C11 P1 Ni1 116.30(12) . .
S1 P1 Ni1 51.70(4) . .
S2 P1 Ni1 51.86(4) . .
C16 C11 C12 119.8(3) . .
C16 C11 P1 120.3(3) . .
C12 C11 P1 119.9(3) . .
C13 C12 C11 120.2(4) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C12 C13 C14 119.8(4) . .
C12 C13 H13 120.1 . .
C14 C13 H13 120.1 . .
C15 C14 C13 120.3(4) . .
C15 C14 C17 120.8(4) . .
C13 C14 C17 118.8(4) . .
C14 C15 C16 120.0(4) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C11 119.9(4) . .
C15 C16 H16 120.1 . .
C11 C16 H16 120.1 . .
F11 C17 F13 107.4(4) . .
F11 C17 F12 106.2(4) . .
F13 C17 F12 105.0(4) . .
F11 C17 C14 113.5(4) . .
F13 C17 C14 112.0(3) . .
F12 C17 C14 112.2(4) . .
C26 C21 C22 119.7(3) . .
C26 C21 P1 121.7(3) . .
C22 C21 P1 118.6(3) . .
C23 C22 C21 119.8(4) . .
C23 C22 H22 120.1 . .
C21 C22 H22 120.1 . .
C24 C23 C22 120.2(4) . .
C24 C23 H23 119.9 . .
C22 C23 H23 119.9 . .
C25 C24 C23 120.5(4) . .
C25 C24 C27 119.9(4) . .
C23 C24 C27 119.6(4) . .
C24 C25 C26 119.5(4) . .
C24 C25 H25 120.3 . .
C26 C25 H25 120.3 . .
C21 C26 C25 120.3(4) . .
C21 C26 H26 119.8 . .
C25 C26 H26 119.8 . .
F21B C27 F22A 125.5(7) . .
F21B C27 F23A 52.0(5) . .
F22A C27 F23A 112.3(5) . .
F21B C27 F23B 110.5(6) . .
F22A C27 F23B 32.9(5) . .
F23A C27 F23B 130.1(7) . .
F21B C27 F22B 102.7(6) . .
F22A C27 F22B 69.5(5) . .
F23A C27 F22B 53.5(5) . .
F23B C27 F22B 101.2(5) . .
F21B C27 F21A 49.4(6) . .
F22A C27 F21A 103.2(5) . .
F23A C27 F21A 100.6(5) . .
F23B C27 F21A 72.8(5) . .
F22B C27 F21A 141.6(6) . .
F21B C27 C24 118.2(5) . .
F22A C27 C24 115.3(5) . .
F23A C27 C24 113.8(5) . .
F23B C27 C24 114.8(6) . .
F22B C27 C24 107.0(5) . .
F21A C27 C24 109.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S1 2.2324(12) .
Ni1 S1 2.2324(12) 3_775
Ni1 S2 2.2389(14) .
Ni1 S2 2.2389(13) 3_775
Ni1 P1 2.8258(15) 3_775
Ni1 P1 2.8258(15) .
S1 P1 2.0066(15) .
S2 P1 2.0146(15) .
P1 C21 1.803(4) .
P1 C11 1.807(4) .
C11 C16 1.390(5) .
C11 C12 1.392(5) .
C12 C13 1.381(5) .
C12 H12 0.9300 .
C13 C14 1.391(5) .
C13 H13 0.9300 .
C14 C15 1.380(5) .
C14 C17 1.492(6) .
C15 C16 1.389(6) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 F11 1.320(5) .
C17 F13 1.334(5) .
C17 F12 1.344(5) .
C21 C26 1.383(5) .
C21 C22 1.387(5) .
C22 C23 1.383(6) .
C22 H22 0.9300 .
C23 C24 1.379(6) .
C23 H23 0.9300 .
C24 C25 1.376(6) .
C24 C27 1.494(6) .
C25 C26 1.390(5) .
C25 H25 0.9300 .
C26 H26 0.9300 .
C27 F21B 1.285(5) .
C27 F22A 1.296(5) .
C27 F23A 1.296(5) .
C27 F23B 1.305(5) .
C27 F22B 1.372(5) .
C27 F21A 1.380(5) .
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 34.4(3)
C22 C21 P1 S1 40.5(3)
