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#$Date: 2019-11-28 13:54:58 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243903 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/25/7702550.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_7702550
loop_
_publ_author_name
'Aragoni, M. Carla'
'Arca, Massimiliano'
'Demartin, Francesco'
'Devillanova, Francesco A.'
'Graiff, Claudia'
'Isaia, Francesco'
'Lippolis, Vito'
'Tiripicchio, Antonio'
'Verani, Gaetano'
_publ_section_title
;
 Reactivity of phosphonodithioato NiII complexes: solution equilibria,
 solid state studies and theoretical calculations on the adduct formation
 with some pyridine derivatives†
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2671
_journal_paper_doi               10.1039/b100991p
_journal_year                    2001
_chemical_formula_sum            'C26 H30 N2 Ni O4 P2 S4'
_chemical_formula_weight         683.41
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.70(2)
_cell_angle_beta                 76.59(3)
_cell_angle_gamma                82.95(3)
_cell_formula_units_Z            1
_cell_length_a                   6.944(2)
_cell_length_b                   9.295(2)
_cell_length_c                   12.503(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.2
_cell_measurement_theta_min      10.4
_cell_volume                     758.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'CAD 4'
_diffrn_measurement_method       omega/2theta
_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  0.0130
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2443
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         3.02
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   'semiempirical (psi-scan)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             354
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0360
_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)+(0.0525P)²+0.3311P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                1809
_reflns_number_total             2443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100991p.txt
_cod_data_source_block           COMPOUND_(7)
_cod_database_code               7702550
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.0000 0.0000 0.0000 0.0305(2) Uani 1 2 d S
S2 S -0.17562(12) 0.19232(9) -0.12851(8) 0.0381(2) Uani 1 1 d .
S1 S 0.26560(13) 0.02176(9) -0.17587(8) 0.0406(3) Uani 1 1 d .
P1 P 0.07455(13) 0.17460(9) -0.24312(8) 0.0344(2) Uani 1 1 d .
O2 O 0.3987(4) 0.7682(3) -0.4390(3) 0.0647(8) Uani 1 1 d .
O1 O 0.0249(4) 0.1426(3) -0.3533(2) 0.0471(7) Uani 1 1 d .
N1 N 0.1141(4) 0.1734(3) 0.0453(2) 0.0342(7) Uani 1 1 d .
C1 C 0.1820(5) 0.3502(4) -0.3047(3) 0.0355(8) Uani 1 1 d .
C2 C 0.3620(5) 0.3772(4) -0.2861(3) 0.0463(10) Uani 1 1 d .
H2 H 0.4317 0.3015 -0.2435 0.056 Uiso 1 1 calc R
C3 C 0.4399(6) 0.5151(4) -0.3298(3) 0.0500(10) Uani 1 1 d .
H3 H 0.5611 0.5313 -0.3167 0.060 Uiso 1 1 calc R
C4 C 0.3375(6) 0.6283(4) -0.3927(3) 0.0464(10) Uani 1 1 d .
C5 C 0.1578(6) 0.6032(4) -0.4136(3) 0.0473(10) Uani 1 1 d .
H5 H 0.0893 0.6787 -0.4571 0.057 Uiso 1 1 calc R
C6 C 0.0820(5) 0.4658(4) -0.3694(3) 0.0426(9) Uani 1 1 d .
H6 H -0.0389 0.4498 -0.3830 0.051 Uiso 1 1 calc R
C7 C 0.5784(7) 0.8010(5) -0.4176(5) 0.0780(15) Uani 1 1 d .
H7A H 0.6053 0.9023 -0.4545 0.117 Uiso 1 1 calc R
H7B H 0.6852 0.7355 -0.4462 0.117 Uiso 1 1 calc R
H7C H 0.5665 0.7875 -0.3378 0.117 Uiso 1 1 calc R
C13 C -0.0074(5) 0.2806(4) 0.0859(3) 0.0405(9) Uani 1 1 d .
H13 H -0.1432 0.2783 0.0925 0.049 Uiso 1 1 calc R
C12 C 0.0586(6) 0.3931(4) 0.1181(3) 0.0477(10) Uani 1 1 d .
H12 H -0.0311 0.4652 0.1454 0.057 Uiso 1 1 calc R
C11 C 0.2578(6) 0.3983(4) 0.1098(4) 0.0523(10) Uani 1 1 d .
H11 H 0.3062 0.4729 0.1318 0.063 Uiso 1 1 calc R
C10 C 0.3836(6) 0.2905(4) 0.0680(4) 0.0566(11) Uani 1 1 d .
H10 H 0.5199 0.2915 0.0603 0.068 Uiso 1 1 calc R
C9 C 0.3078(5) 0.1812(4) 0.0377(3) 0.0452(10) Uani 1 1 d .
H9 H 0.3957 0.1083 0.0102 0.054 Uiso 1 1 calc R
C8 C -0.0902(8) 0.0201(5) -0.3436(4) 0.0690(14) Uani 1 1 d .
H8A H -0.1067 0.0167 -0.4171 0.104 Uiso 1 1 calc R
H8B H -0.2180 0.0329 -0.2958 0.104 Uiso 1 1 calc R
H8C H -0.0229 -0.0712 -0.3114 0.104 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
Ni Ni 0.3393 1.1124 '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'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N1 Ni N1 180.00(14) . 2
N1 Ni S2 89.00(8) . .
N1 Ni S2 91.00(8) 2 .
N1 Ni S2 91.00(8) . 2
N1 Ni S2 89.00(8) 2 2
S2 Ni S2 180.00(3) . 2
N1 Ni S1 90.90(8) . .
N1 Ni S1 89.10(8) 2 .
S2 Ni S1 81.68(4) . .
S2 Ni S1 98.32(4) 2 .
N1 Ni S1 89.10(8) . 2
N1 Ni S1 90.90(8) 2 2
S2 Ni S1 98.32(4) . 2
S2 Ni S1 81.68(4) 2 2
S1 Ni S1 180.00(5) . 2
P1 S2 Ni 84.08(5) . .
P1 S1 Ni 84.02(5) . .
O1 P1 C1 99.10(15) . .
O1 P1 S1 113.18(11) . .
C1 P1 S1 111.75(12) . .
O1 P1 S2 109.96(11) . .
C1 P1 S2 112.27(12) . .
S1 P1 S2 110.19(6) . .
C4 O2 C7 117.4(3) . .
C8 O1 P1 120.1(2) . .
C9 N1 C13 116.1(3) . .
C9 N1 Ni 122.7(2) . .
C13 N1 Ni 121.2(2) . .
C2 C1 C6 117.9(3) . .
C2 C1 P1 121.5(3) . .
C6 C1 P1 120.5(3) . .
C1 C2 C3 121.2(3) . .
C4 C3 C2 119.9(4) . .
O2 C4 C3 125.0(4) . .
O2 C4 C5 115.1(3) . .
C3 C4 C5 119.9(3) . .
C6 C5 C4 119.6(3) . .
C5 C6 C1 121.5(3) . .
N1 C13 C12 123.4(3) . .
C11 C12 C13 119.3(4) . .
C10 C11 C12 118.1(4) . .
C9 C10 C11 119.6(4) . .
N1 C9 C10 123.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni N1 2.125(3) .
Ni N1 2.125(3) 2
Ni S2 2.4938(12) .
Ni S2 2.4938(12) 2
Ni S1 2.5036(13) .
Ni S1 2.5036(13) 2
S2 P1 1.9975(14) .
S1 P1 1.9874(14) .
P1 O1 1.598(3) .
P1 C1 1.796(3) .
O2 C4 1.362(4) .
O2 C7 1.418(5) .
O1 C8 1.435(5) .
N1 C9 1.336(4) .
N1 C13 1.345(4) .
C1 C2 1.385(5) .
C1 C6 1.392(5) .
C2 C3 1.386(5) .
C3 C4 1.377(5) .
C4 C5 1.390(5) .
C5 C6 1.377(5) .
C13 C12 1.370(5) .
C12 C11 1.369(5) .
C11 C10 1.368(5) .
C10 C9 1.367(5) .
