#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/96/4329616.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_4329616
loop_
_publ_author_name
'Dimitrios Maganas'
'J. Krzystek'
'Eleftherios Ferentinos'
'Alexander M. Whyte'
'Neil Robertson'
'Vassilis Psycharis'
'Aris Terzis'
'Frank Neese'
'Panayotis Kyritsis'
_publ_section_title
;
 Investigating Magnetostructural Correlations in the Pseudooctahedral
 trans-[NiII{(OPPh2)(EPPh2)N}2(sol)2] Complexes (E = S, Se; sol = DMF,
 THF) by Magnetometry, HFEPR, and ab Initio Quantum Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7218
_journal_page_last               7231
_journal_paper_doi               10.1021/ic300453y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C14 H14 N0.5 Ni0.25 O P S0.5'
_chemical_formula_weight         266.93
_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                 105.4250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.7934(2)
_cell_length_b                   9.49580(10)
_cell_length_c                   20.7500(3)
_cell_measurement_reflns_used    15174
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      133.90
_cell_measurement_theta_min      13.10
_cell_volume                     2619.92(6)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15977
_diffrn_reflns_theta_full        64.99
_diffrn_reflns_theta_max         64.99
_diffrn_reflns_theta_min         6.45
_exptl_absorpt_coefficient_mu    2.813
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       parallelepide
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         4294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0777P)²+2.4573P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                3759
_reflns_number_total             4294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300453y_si_002_1.cif
_cod_data_source_block           kyniosthf
_cod_original_formula_sum        'C14 H14 N0.50 Ni0.25 O P S0.50'
_cod_database_code               4329616
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
Ni Ni 0.5000 0.5000 0.0000 0.0241(2) Uani 1 2 d S
O O 0.60649(14) 0.4544(2) -0.04694(10) 0.0323(5) Uani 1 1 d .
S S 0.62045(5) 0.60584(8) 0.10262(4) 0.0327(2) Uani 1 1 d .
N N 0.77935(17) 0.5877(2) 0.02003(12) 0.0291(5) Uani 1 1 d .
P1 P 0.71406(5) 0.50063(7) -0.04335(3) 0.0259(2) Uani 1 1 d .
P2 P 0.76100(5) 0.62125(7) 0.09173(3) 0.0264(2) Uani 1 1 d .
C1 C 0.7847(2) 0.3437(3) -0.05437(14) 0.0288(6) Uani 1 1 d .
C2 C 0.7319(2) 0.2253(3) -0.08732(15) 0.0355(7) Uani 1 1 d .
C3 C 0.7847(3) 0.1085(4) -0.10103(17) 0.0459(9) Uani 1 1 d .
C4 C 0.8906(3) 0.1089(4) -0.08186(17) 0.0462(9) Uani 1 1 d .
C5 C 0.9435(3) 0.2246(3) -0.04814(17) 0.0414(8) Uani 1 1 d .
C6 C 0.8911(2) 0.3414(3) -0.03429(16) 0.0353(7) Uani 1 1 d .
C7 C 0.7118(2) 0.6052(3) -0.11752(14) 0.0310(7) Uani 1 1 d .
C8 C 0.6282(3) 0.5925(4) -0.17467(17) 0.0515(9) Uani 1 1 d .
C9 C 0.6269(3) 0.6682(5) -0.2332(2) 0.0655(12) Uani 1 1 d .
C10 C 0.7069(3) 0.7548(4) -0.23497(18) 0.0520(10) Uani 1 1 d .
C11 C 0.7896(3) 0.7687(3) -0.17837(17) 0.0451(8) Uani 1 1 d .
C12 C 0.7919(3) 0.6940(3) -0.12013(16) 0.0378(7) Uani 1 1 d .
C21 C 0.8488(2) 0.5165(3) 0.15681(15) 0.0310(7) Uani 1 1 d .
C22 C 0.8177(3) 0.4413(3) 0.20564(15) 0.0383(7) Uani 1 1 d .
C23 C 0.8893(3) 0.3668(4) 0.25573(17) 0.0481(9) Uani 1 1 d .
C24 C 0.9902(3) 0.3669(3) 0.25765(17) 0.0487(10) Uani 1 1 d .
C25 C 1.0220(3) 0.4431(4) 0.20970(19) 0.0475(9) Uani 1 1 d .
C26 C 0.9520(3) 0.5167(3) 0.15960(18) 0.0402(8) Uani 1 1 d .
C27 C 0.8073(2) 0.8010(3) 0.11262(14) 0.0283(6) Uani 1 1 d .
C28 C 0.8391(2) 0.8480(3) 0.17954(15) 0.0348(7) Uani 1 1 d .
C29 C 0.8727(3) 0.9858(3) 0.19520(17) 0.0402(8) Uani 1 1 d .
C30 C 0.8761(2) 1.0792(3) 0.14405(17) 0.0393(7) Uani 1 1 d .
C31 C 0.8451(2) 1.0350(3) 0.07757(17) 0.0344(7) Uani 1 1 d .
C32 C 0.8108(2) 0.8969(3) 0.06146(15) 0.0292(6) Uani 1 1 d .
O41 O 0.52408(14) 0.2973(2) 0.04782(10) 0.0317(5) Uani 1 1 d .
C41 C 0.6211(2) 0.2251(3) 0.06830(17) 0.0375(7) Uani 1 1 d .
C42 C 0.6085(3) 0.1147(4) 0.1189(2) 0.0474(9) Uani 1 1 d .
C43 C 0.4931(3) 0.0889(4) 0.10127(19) 0.0448(8) Uani 1 1 d .
C44 C 0.4494(2) 0.1867(3) 0.04164(17) 0.0359(7) Uani 1 1 d .
H2 H 0.658(3) 0.225(4) -0.0992(17) 0.050(10) Uiso 1 1 d .
H3 H 0.748(3) 0.035(4) -0.1235(19) 0.052(11) Uiso 1 1 d .
H4 H 0.926(3) 0.035(4) -0.0870(19) 0.055(11) Uiso 1 1 d .
H5 H 1.016(3) 0.223(4) -0.0349(17) 0.045(9) Uiso 1 1 d .
H6 H 0.928(3) 0.421(4) -0.0098(17) 0.045(9) Uiso 1 1 d .
H8 H 0.567(3) 0.527(4) -0.173(2) 0.064(12) Uiso 1 1 d .
H9 H 0.561(3) 0.661(5) -0.275(2) 0.081(14) Uiso 1 1 d .
H10 H 0.709(3) 0.803(4) -0.271(2) 0.060(11) Uiso 1 1 d .
H11 H 0.846(3) 0.820(4) -0.1793(17) 0.046(10) Uiso 1 1 d .
H12 H 0.847(3) 0.704(4) -0.0824(18) 0.045(10) Uiso 1 1 d .
H22 H 0.745(3) 0.438(3) 0.1997(15) 0.033(8) Uiso 1 1 d .
H23 H 0.864(3) 0.318(4) 0.2843(18) 0.045(10) Uiso 1 1 d .
H24 H 1.042(3) 0.316(4) 0.294(2) 0.068(12) Uiso 1 1 d .
H25 H 1.086(4) 0.456(5) 0.208(2) 0.091(17) Uiso 1 1 d .
H26 H 0.973(3) 0.570(5) 0.127(2) 0.082(14) Uiso 1 1 d .
H28 H 0.835(2) 0.774(4) 0.2145(17) 0.042(9) Uiso 1 1 d .
H29 H 0.897(3) 1.020(4) 0.240(2) 0.063(12) Uiso 1 1 d .
H30 H 0.901(3) 1.180(4) 0.1511(17) 0.047(10) Uiso 1 1 d .
H31 H 0.846(3) 1.091(4) 0.0453(19) 0.049(11) Uiso 1 1 d .
H32 H 0.789(2) 0.864(3) 0.0154(16) 0.032(8) Uiso 1 1 d .
H41A H 0.676(2) 0.298(4) 0.0846(16) 0.040(9) Uiso 1 1 d .
H41B H 0.634(3) 0.174(4) 0.0292(19) 0.052(10) Uiso 1 1 d .
H42A H 0.654(4) 0.023(5) 0.115(2) 0.091(16) Uiso 1 1 d .
H42B H 0.630(4) 0.164(5) 0.160(3) 0.086(15) Uiso 1 1 d .
H43A H 0.476(3) -0.014(4) 0.0906(19) 0.060(12) Uiso 1 1 d .
H43B H 0.469(3) 0.125(4) 0.138(2) 0.058(11) Uiso 1 1 d .
H44A H 0.384(2) 0.236(3) 0.0412(16) 0.039(9) Uiso 1 1 d .
H44B H 0.437(3) 0.135(4) -0.005(2) 0.059(11) Uiso 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 0.0181 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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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'
Ni Ni -3.0029 0.5091 '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
O Ni O 180.00(9) . 3_665
O Ni O41 90.69(8) . 3_665
O Ni O41 89.31(8) 3_665 3_665
O Ni O41 89.31(8) . .
O Ni O41 90.69(8) 3_665 .
O41 Ni O41 180.00(10) 3_665 .
O Ni S 84.71(6) . 3_665
O Ni S 95.29(6) 3_665 3_665
O41 Ni S 88.91(5) 3_665 3_665
O41 Ni S 91.09(5) . 3_665
O Ni S 95.29(6) . .
O Ni S 84.71(6) 3_665 .
O41 Ni S 91.09(5) 3_665 .
O41 Ni S 88.91(5) . .
S Ni S 180.00(2) 3_665 .
P1 O Ni 137.53(13) . .
P2 S Ni 111.69(4) . .
P2 N P1 131.81(16) . .
O P1 N 120.76(12) . .
O P1 C7 108.41(13) . .
N P1 C7 106.86(13) . .
O P1 C1 107.60(12) . .
N P1 C1 108.65(13) . .
C7 P1 C1 103.21(13) . .
N P2 C27 105.83(13) . .
N P2 C21 109.66(13) . .
C27 P2 C21 102.06(13) . .
N P2 S 118.86(9) . .
C27 P2 S 109.04(9) . .
C21 P2 S 110.00(10) . .
C2 C1 C6 119.4(3) . .
C2 C1 P1 119.1(2) . .
C6 C1 P1 121.4(2) . .
C3 C2 C1 120.0(3) . .
C3 C2 H2 121(2) . .
C1 C2 H2 119(2) . .
C2 C3 C4 119.9(3) . .
C2 C3 H3 117(2) . .
C4 C3 H3 123(2) . .
C5 C4 C3 120.5(3) . .
C5 C4 H4 117(3) . .
C3 C4 H4 123(3) . .
C6 C5 C4 119.8(3) . .
C6 C5 H5 121(2) . .
C4 C5 H5 119(2) . .
C5 C6 C1 120.3(3) . .
C5 C6 H6 120(2) . .
C1 C6 H6 120(2) . .
C12 C7 C8 119.4(3) . .
C12 C7 P1 121.5(2) . .
C8 C7 P1 119.1(3) . .
C9 C8 C7 119.9(4) . .
C9 C8 H8 120(2) . .
C7 C8 H8 120(2) . .
C10 C9 C8 120.0(4) . .
C10 C9 H9 121(2) . .
C8 C9 H9 118(2) . .
C9 C10 C11 120.5(3) . .
C9 C10 H10 123(3) . .
C11 C10 H10 117(3) . .
C12 C11 C10 120.0(4) . .
C12 C11 H11 117(2) . .
C10 C11 H11 122(2) . .
C11 C12 C7 120.2(3) . .
C11 C12 H12 120(2) . .
C7 C12 H12 120(2) . .
C22 C21 C26 118.2(3) . .
C22 C21 P2 122.5(2) . .
C26 C21 P2 119.2(2) . .
C21 C22 C23 119.9(3) . .
C21 C22 H22 115.3(18) . .
C23 C22 H22 124.6(19) . .
C24 C23 C22 121.4(3) . .
C24 C23 H23 124(2) . .
C22 C23 H23 115(2) . .
C23 C24 C25 119.1(3) . .
C23 C24 H24 122(2) . .
C25 C24 H24 119(2) . .
C24 C25 C26 120.2(4) . .
C24 C25 H25 127(3) . .
C26 C25 H25 113(3) . .
C25 C26 C21 121.2(3) . .
C25 C26 H26 121(3) . .
C21 C26 H26 118(3) . .
C32 C27 C28 118.2(3) . .
C32 C27 P2 120.2(2) . .
C28 C27 P2 121.6(2) . .
C29 C28 C27 121.4(3) . .
C29 C28 H28 123.8(19) . .
C27 C28 H28 114.8(19) . .
C30 C29 C28 119.7(3) . .
C30 C29 H29 117(2) . .
C28 C29 H29 123(2) . .
C29 C30 C31 119.9(3) . .
C29 C30 H30 125(2) . .
C31 C30 H30 115(2) . .
C30 C31 C32 120.7(3) . .
C30 C31 H31 121(2) . .
C32 C31 H31 118(2) . .
C31 C32 C27 120.1(3) . .
C31 C32 H32 122.1(18) . .
C27 C32 H32 117.8(18) . .
C44 O41 C41 105.0(2) . .
C44 O41 Ni 125.99(16) . .
C41 O41 Ni 124.79(17) . .
O41 C41 C42 105.0(3) . .
O41 C41 H41A 109.1(19) . .
C42 C41 H41A 116.7(18) . .
O41 C41 H41B 110(2) . .
C42 C41 H41B 108(2) . .
H41A C41 H41B 109(3) . .
C41 C42 C43 104.1(3) . .
C41 C42 H42A 109(3) . .
C43 C42 H42A 116(3) . .
C41 C42 H42B 102(3) . .
C43 C42 H42B 110(3) . .
H42A C42 H42B 114(4) . .
C44 C43 C42 104.6(3) . .
C44 C43 H43A 113(2) . .
C42 C43 H43A 111(2) . .
C44 C43 H43B 106(2) . .
C42 C43 H43B 108(2) . .
H43A C43 H43B 114(3) . .
O41 C44 C43 104.4(2) . .
O41 C44 H44A 106.1(19) . .
C43 C44 H44A 116.3(19) . .
O41 C44 H44B 111(2) . .
C43 C44 H44B 113(2) . .
H44A C44 H44B 106(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni O 2.014(2) .
Ni O 2.014(2) 3_665
Ni O41 2.1507(18) 3_665
Ni O41 2.1507(18) .
Ni S 2.5343(7) 3_665
Ni S 2.5343(7) .
O P1 1.530(2) .
S P2 2.0160(10) .
N P2 1.606(2) .
N P1 1.611(2) .
P1 C7 1.825(3) .
P1 C1 1.828(3) .
P2 C27 1.834(3) .
P2 C21 1.846(3) .
C1 C2 1.413(4) .
C1 C6 1.416(4) .
C2 C3 1.397(5) .
C2 H2 0.98(4) .
C3 C4 1.407(5) .
C3 H3 0.91(4) .
C4 C5 1.399(5) .
C4 H4 0.88(4) .
C5 C6 1.395(5) .
C5 H5 0.96(4) .
C6 H6 0.98(4) .
C7 C12 1.403(4) .
C7 C8 1.422(4) .
C8 C9 1.407(5) .
C8 H8 1.06(4) .
C9 C10 1.384(6) .
C9 H9 1.08(5) .
C10 C11 1.409(5) .
C10 H10 0.89(4) .
C11 C12 1.395(4) .
C11 H11 0.92(4) .
C12 H12 0.94(3) .
C21 C22 1.397(4) .
C21 C26 1.410(5) .
C22 C23 1.418(5) .
C22 H22 0.98(3) .
C23 C24 1.381(6) .
C23 H23 0.89(4) .
C24 C25 1.393(6) .
C24 H24 1.01(4) .
C25 C26 1.402(5) .
C25 H25 0.91(5) .
C26 H26 0.95(5) .
C27 C32 1.409(4) .
C27 C28 1.413(4) .
C28 C29 1.397(4) .
C28 H28 1.02(3) .
C29 C30 1.393(5) .
C29 H29 0.97(4) .
C30 C31 1.396(5) .
C30 H30 1.01(4) .
C31 C32 1.404(4) .
C31 H31 0.86(4) .
C32 H32 0.98(3) .
O41 C44 1.453(4) .
O41 C41 1.463(4) .
C41 C42 1.526(5) .
C41 H41A 1.02(3) .
C41 H41B 1.00(4) .
C42 C43 1.555(5) .
C42 H42A 1.09(5) .
C42 H42B 0.94(5) .
C43 C44 1.536(4) .
C43 H43A 1.02(4) .
C43 H43B 0.97(4) .
C44 H44A 1.01(3) .
C44 H44B 1.05(4) .
