#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179399 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/96/4329687.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_4329687
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                 95.952(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.179(3)
_cell_length_b                   7.876(3)
_cell_length_c                   20.948(7)
_cell_measurement_temperature    120(1)
_cell_volume                     1506.2(9)
_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 0.996
_diffrn_measured_fraction_theta_max 0.991
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4055
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.9564
_exptl_absorpt_correction_T_min  0.7290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0515
_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)+(0.1171P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                3546
_reflns_number_total             4146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3001587_si_003_1.cif
_cod_data_source_block           apx1150_hklf5_nis2_ocf3
_cod_original_cell_volume        1506.1(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329687
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
Ni1 Ni 0.5000 1.0000 0.0000 0.0147(2) Uani 1 2 d S
S1 S 0.59979(13) 0.74414(14) -0.00157(5) 0.0173(3) Uani 1 1 d .
S2 S 0.62453(15) 1.03852(14) 0.09552(5) 0.0192(3) Uani 1 1 d .
P1 P 0.70314(14) 0.80243(15) 0.08531(5) 0.0149(3) Uani 1 1 d .
C11 C 0.9022(5) 0.7950(6) 0.0858(2) 0.0169(10) Uani 1 1 d .
C12 C 0.9706(6) 0.9505(6) 0.0835(2) 0.0203(11) Uani 1 1 d .
H12 H 0.9146 1.0491 0.0822 0.024 Uiso 1 1 calc R
C13 C 1.1212(6) 0.9625(6) 0.0830(2) 0.0191(11) Uani 1 1 d .
H13 H 1.1653 1.0683 0.0807 0.023 Uiso 1 1 calc R
C14 C 1.2046(6) 0.8180(6) 0.0859(2) 0.0214(11) Uani 1 1 d .
H14 H 1.3058 0.8257 0.0862 0.026 Uiso 1 1 calc R
C15 C 1.1392(5) 0.6624(6) 0.0882(2) 0.0198(11) Uani 1 1 d .
H15 H 1.1967 0.5650 0.0901 0.024 Uiso 1 1 calc R
C16 C 0.9874(6) 0.6476(6) 0.0877(2) 0.0180(10) Uani 1 1 d .
C17 C 0.9263(6) 0.4705(6) 0.0866(2) 0.0190(10) Uani 1 1 d .
F11 F 0.7985(3) 0.4593(3) 0.04943(12) 0.0211(6) Uani 1 1 d .
F12 F 0.9013(3) 0.4153(3) 0.14521(12) 0.0229(7) Uani 1 1 d .
F13 F 1.0162(3) 0.3576(3) 0.06413(12) 0.0224(7) Uani 1 1 d .
C21 C 0.6545(5) 0.6593(6) 0.1482(2) 0.0167(10) Uani 1 1 d .
C22 C 0.5482(5) 0.5389(6) 0.1290(2) 0.0164(10) Uani 1 1 d .
H22 H 0.5030 0.5404 0.0872 0.020 Uiso 1 1 calc R
C23 C 0.5089(6) 0.4167(6) 0.1716(2) 0.0244(11) Uani 1 1 d .
H23 H 0.4381 0.3364 0.1579 0.029 Uiso 1 1 calc R
C24 C 0.5731(6) 0.4127(7) 0.2335(2) 0.0310(13) Uani 1 1 d .
H24 H 0.5470 0.3295 0.2617 0.037 Uiso 1 1 calc R
C25 C 0.6767(6) 0.5329(6) 0.2537(2) 0.0248(12) Uani 1 1 d .
H25 H 0.7191 0.5315 0.2960 0.030 Uiso 1 1 calc R
C26 C 0.7189(6) 0.6563(6) 0.2120(2) 0.0203(11) Uani 1 1 d .
C27 C 0.8344(6) 0.7795(6) 0.2397(2) 0.0221(11) Uani 1 1 d .
F21 F 0.8230(4) 0.9316(4) 0.21162(13) 0.0289(7) Uani 1 1 d .
F22 F 0.9693(3) 0.7220(4) 0.23488(13) 0.0292(7) Uani 1 1 d .
F23 F 0.8238(3) 0.8065(4) 0.30193(12) 0.0316(8) Uani 1 1 d .
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_675
S1 Ni1 S2 92.14(4) . 3_675
S1 Ni1 S2 87.86(4) 3_675 3_675
S1 Ni1 S2 87.86(4) . .
S1 Ni1 S2 92.14(4) 3_675 .
S2 Ni1 S2 179.999(1) 3_675 .
P1 S1 Ni1 86.34(5) . .
P1 S2 Ni1 86.26(5) . .
C21 P1 C11 107.2(2) . .
C21 P1 S2 112.10(16) . .
C11 P1 S2 113.46(16) . .
C21 P1 S1 112.58(16) . .
C11 P1 S1 112.00(15) . .
S2 P1 S1 99.55(7) . .
C12 C11 C16 118.9(5) . .
C12 C11 P1 115.4(4) . .
C16 C11 P1 125.6(4) . .
C11 C12 C13 121.2(5) . .
C11 C12 H12 119.4 . .
C13 C12 H12 119.4 . .
C14 C13 C12 119.8(5) . .
C14 C13 H13 120.1 . .
C12 C13 H13 120.1 . .
C13 C14 C15 120.1(5) . .
C13 C14 H14 120.0 . .
C15 C14 H14 120.0 . .
C14 C15 C16 121.0(5) . .
C14 C15 H15 119.5 . .
C16 C15 H15 119.5 . .
C15 C16 C11 119.0(4) . .
C15 C16 C17 116.6(4) . .
C11 C16 C17 124.3(4) . .
F13 C17 F12 106.1(4) . .
F13 C17 F11 106.7(4) . .
F12 C17 F11 106.7(4) . .
F13 C17 C16 112.4(4) . .
F12 C17 C16 112.7(4) . .
F11 C17 C16 111.8(4) . .
C22 C21 C26 118.6(4) . .
C22 C21 P1 115.4(3) . .
C26 C21 P1 126.0(4) . .
C23 C22 C21 120.6(4) . .
C23 C22 H22 119.7 . .
C21 C22 H22 119.7 . .
C24 C23 C22 120.8(5) . .
C24 C23 H23 119.6 . .
C22 C23 H23 119.6 . .
C23 C24 C25 119.4(5) . .
C23 C24 H24 120.3 . .
C25 C24 H24 120.3 . .
C24 C25 C26 121.1(5) . .
C24 C25 H25 119.5 . .
C26 C25 H25 119.5 . .
C25 C26 C21 119.5(5) . .
C25 C26 C27 116.0(4) . .
C21 C26 C27 124.5(4) . .
F22 C27 F21 107.7(4) . .
F22 C27 F23 106.9(4) . .
F21 C27 F23 106.1(4) . .
F22 C27 C26 111.9(4) . .
F21 C27 C26 112.8(4) . .
F23 C27 C26 111.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S1 2.2151(13) .
Ni1 S1 2.2151(13) 3_675
Ni1 S2 2.2199(13) 3_675
Ni1 S2 2.2200(13) .
S1 P1 2.0161(16) .
S2 P1 2.0138(17) .
P1 C21 1.825(5) .
P1 C11 1.827(5) .
C11 C12 1.379(7) .
C11 C16 1.398(7) .
C12 C13 1.386(7) .
C12 H12 0.9300 .
C13 C14 1.369(7) .
C13 H13 0.9300 .
C14 C15 1.368(7) .
C14 H14 0.9300 .
C15 C16 1.398(7) .
C15 H15 0.9300 .
C16 C17 1.502(6) .
C17 F13 1.331(5) .
C17 F12 1.344(5) .
C17 F11 1.343(5) .
C21 C22 1.390(7) .
C21 C26 1.403(6) .
C22 C23 1.385(7) .
C22 H22 0.9300 .
C23 C24 1.369(7) .
C23 H23 0.9300 .
C24 C25 1.377(8) .
C24 H24 0.9300 .
C25 C26 1.390(7) .
C25 H25 0.9300 .
C26 C27 1.508(7) .
C27 F22 1.332(6) .
C27 F21 1.334(6) .
C27 F23 1.334(5) .
