#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:27:31 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179791 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/87/7008785.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_7008785
loop_
_publ_author_name
'Chang, Xiaohong'
'Lee, Kyung-Eun'
'Il Jeon, Sang'
'Kim, Yong-Joo'
'Lee, H.-K.'
'Lee, Soon W.'
_publ_section_title
;
 Bis(isothiocyanato)bis(phosphine) complexes of group 10 metals:
 reactivity toward organic isocyanides
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              3722
_journal_paper_doi               10.1039/b508134c
_journal_year                    2005
_chemical_formula_sum            'C27 H31 N3 Ni P2 S2'
_chemical_formula_weight         582.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.503(3)
_cell_length_b                   12.9769(15)
_cell_length_c                   15.918(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.88
_cell_measurement_theta_min      5.07
_cell_volume                     2995.8(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2731
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_T_max  0.5935
_exptl_absorpt_correction_T_min  0.5501
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'RED '
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'BLOCK '
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1722
_refine_ls_R_factor_gt           0.0661
_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)+(0.0420P)²+2.6601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                1188
_reflns_number_total             2731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508134c.txt
_cod_data_source_block           nincs2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2995.9(9)
_cod_original_sg_symbol_H-M      'Pnma '
_cod_database_code               7008785
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.68690(9) 0.2500 0.42136(7) 0.0567(4) Uani 1 2 d S . .
S1 S 0.8641(3) 0.2500 0.6631(2) 0.166(2) Uani 1 2 d S . .
S2 S 0.4413(2) 0.2500 0.62069(18) 0.0873(10) Uani 1 2 d S . .
P1 P 0.68224(14) 0.07995(14) 0.41784(12) 0.0680(6) Uani 1 1 d . . .
N1 N 0.6659(5) 0.2500 0.2380(5) 0.062(2) Uani 1 2 d S . .
N2 N 0.7679(6) 0.2500 0.5152(5) 0.082(3) Uani 1 2 d S . .
N3 N 0.5619(7) 0.2500 0.4876(6) 0.101(3) Uani 1 2 d S . .
C1 C 0.6751(7) 0.2500 0.3105(6) 0.062(3) Uani 1 2 d S . .
C2 C 0.6526(8) 0.2500 0.1505(5) 0.061(3) Uani 1 2 d S . .
C3 C 0.5621(9) 0.2500 0.1237(7) 0.072(3) Uani 1 2 d S . .
C4 C 0.5483(10) 0.2500 0.0374(8) 0.097(4) Uani 1 2 d S . .
H4 H 0.4889 0.2500 0.0156 0.117 Uiso 1 2 calc SR . .
C5 C 0.6205(12) 0.2500 -0.0138(8) 0.094(4) Uani 1 2 d S . .
H5 H 0.6091 0.2500 -0.0713 0.113 Uiso 1 2 calc SR . .
C6 C 0.7107(9) 0.2500 0.0121(7) 0.084(4) Uani 1 2 d S . .
H6 H 0.7585 0.2500 -0.0269 0.101 Uiso 1 2 calc SR . .
C7 C 0.7297(8) 0.2500 0.0990(6) 0.072(3) Uani 1 2 d S . .
C8 C 0.4804(8) 0.2500 0.1825(7) 0.102(4) Uani 1 2 d S . .
H8A H 0.4244 0.2500 0.1503 0.153 Uiso 1 2 calc SR . .
H8B H 0.4825 0.3104 0.2173 0.153 Uiso 0.50 1 calc PR . .
H8C H 0.4825 0.1896 0.2173 0.153 Uiso 0.50 1 calc PR . .
C9 C 0.8247(7) 0.2500 0.1352(7) 0.099(4) Uani 1 2 d S . .
H9A H 0.8691 0.2500 0.0905 0.148 Uiso 1 2 calc SR . .
H9B H 0.8330 0.1896 0.1692 0.148 Uiso 0.50 1 calc PR . .
H9C H 0.8330 0.3104 0.1692 0.148 Uiso 0.50 1 calc PR . .
C10 C 0.6746(5) 0.0249(6) 0.5221(4) 0.102(3) Uani 1 1 d . . .
H10A H 0.7282 0.0439 0.5540 0.154 Uiso 1 1 calc R . .
H10B H 0.6712 -0.0488 0.5180 0.154 Uiso 1 1 calc R . .
H10C H 0.6203 0.0504 0.5497 0.154 Uiso 1 1 calc R . .
C11 C 0.5780(5) 0.0350(6) 0.3642(6) 0.120(3) Uani 1 1 d . . .
H11A H 0.5249 0.0680 0.3883 0.179 Uiso 1 1 calc R . .
H11B H 0.5725 -0.0383 0.3707 0.179 Uiso 1 1 calc R . .
H11C H 0.5818 0.0518 0.3056 0.179 Uiso 1 1 calc R . .
C12 C 0.7788(6) 0.0162(6) 0.3712(5) 0.073(2) Uani 1 1 d . . .
C13 C 0.7714(8) -0.0448(6) 0.3001(5) 0.113(3) Uani 1 1 d . . .
H13 H 0.7142 -0.0534 0.2747 0.135 Uiso 1 1 calc R . .
C14 C 0.8483(12) -0.0933(11) 0.2663(8) 0.165(7) Uani 1 1 d . . .
H14 H 0.8417 -0.1354 0.2194 0.198 Uiso 1 1 calc R . .
C15 C 0.9311(11) -0.0799(11) 0.3004(10) 0.154(7) Uani 1 1 d . . .
H15 H 0.9822 -0.1127 0.2773 0.184 Uiso 1 1 calc R . .
C16 C 0.9413(8) -0.0180(9) 0.3697(8) 0.140(4) Uani 1 1 d . . .
H16 H 0.9996 -0.0074 0.3923 0.168 Uiso 1 1 calc R . .
C17 C 0.8652(7) 0.0289(7) 0.4060(6) 0.103(3) Uani 1 1 d . . .
H17 H 0.8724 0.0690 0.4540 0.123 Uiso 1 1 calc R . .
C18 C 0.8080(7) 0.2500 0.5760(7) 0.076(3) Uani 1 2 d S . .
C19 C 0.5126(7) 0.2500 0.5436(6) 0.062(3) Uani 1 2 d S . .
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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
C1 Ni1 N2 147.3(4) . . ?
C1 Ni1 N3 114.6(4) . . ?
N2 Ni1 N3 98.0(4) . . ?
C1 Ni1 P1 88.38(6) . 7_565 ?
N2 Ni1 P1 92.23(7) . 7_565 ?
N3 Ni1 P1 89.21(7) . 7_565 ?
C1 Ni1 P1 88.38(6) . . ?
N2 Ni1 P1 92.23(7) . . ?
N3 Ni1 P1 89.21(7) . . ?
P1 Ni1 P1 175.44(14) 7_565 . ?
C12 P1 C10 104.2(3) . . ?
C12 P1 C11 107.8(4) . . ?
C10 P1 C11 104.5(4) . . ?
C12 P1 Ni1 116.7(3) . . ?
C10 P1 Ni1 111.9(3) . . ?
C11 P1 Ni1 110.8(3) . . ?
C1 N1 C2 178.8(10) . . ?
C18 N2 Ni1 172.8(9) . . ?
C19 N3 Ni1 158.8(10) . . ?
N1 C1 Ni1 178.9(9) . . ?
C3 C2 C7 125.7(9) . . ?
C3 C2 N1 115.9(10) . . ?
C7 C2 N1 118.4(9) . . ?
C2 C3 C4 116.3(12) . . ?
C2 C3 C8 123.7(9) . . ?
C4 C3 C8 120.1(12) . . ?
C5 C4 C3 119.7(13) . . ?
C4 C5 C6 124.6(12) . . ?
C5 C6 C7 118.7(11) . . ?
C2 C7 C6 115.0(10) . . ?
C2 C7 C9 121.0(9) . . ?
C6 C7 C9 123.9(10) . . ?
C17 C12 C13 117.8(9) . . ?
C17 C12 P1 119.3(7) . . ?
C13 C12 P1 122.9(8) . . ?
C12 C13 C14 120.9(11) . . ?
C15 C14 C13 120.5(16) . . ?
C14 C15 C16 120.1(18) . . ?
C15 C16 C17 120.4(14) . . ?
C12 C17 C16 120.2(10) . . ?
N2 C18 S1 179.4(10) . . ?
N3 C19 S2 178.5(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.773(9) . ?
Ni1 N2 1.899(9) . ?
Ni1 N3 2.097(9) . ?
Ni1 P1 2.2084(18) 7_565 ?
Ni1 P1 2.2084(18) . ?
S1 C18 1.608(12) . ?
S2 C19 1.605(11) . ?
P1 C12 1.788(8) . ?
P1 C10 1.811(6) . ?
P1 C11 1.832(7) . ?
N1 C1 1.163(9) . ?
N1 C2 1.405(10) . ?
N2 C18 1.130(11) . ?
N3 C19 1.142(11) . ?
C2 C3 1.380(13) . ?
C2 C7 1.387(13) . ?
C3 C4 1.388(13) . ?
C3 C8 1.509(13) . ?
C4 C5 1.327(15) . ?
C5 C6 1.372(15) . ?
C6 C7 1.410(14) . ?
C7 C9 1.494(13) . ?
C12 C17 1.380(10) . ?
C12 C13 1.385(10) . ?
C13 C14 1.388(14) . ?
C14 C15 1.330(17) . ?
C15 C16 1.372(16) . ?
C16 C17 1.387(12) . ?
