#------------------------------------------------------------------------------
#$Date: 2018-08-09 16:09:44 +0300 (Thu, 09 Aug 2018) $
#$Revision: 209504 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/43/7114381.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_7114381
loop_
_publ_author_name
'Albano, Vincenzo G.'
'Aragoni, M. Carla'
'Arca, Massimiliano'
'Castellari, Carlo'
'Demartin, Francesco'
'Devillanova, Francesco A.'
'Isaia, Francesco'
'Lippolis, Vito'
'Loddo, Laura'
'Verani, Gaetano'
_publ_section_title
;
 An unprecedented example of a cis-phosphonodithioato nickel(ii) complex
 built by an extensive hydrogen bonding supramolecular network
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              1170
_journal_paper_doi               10.1039/b200414c
_journal_year                    2002
_chemical_formula_sum            'C9 H15 N2 O P S2'
_chemical_formula_weight         262.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        '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                 90.240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4077(13)
_cell_length_b                   6.1908(5)
_cell_length_c                   13.7291(12)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      3.2
_cell_volume                     1224.56(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'CCD Smart diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.1323
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16240
_diffrn_reflns_theta_full        32.22
_diffrn_reflns_theta_max         32.22
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   'theta dependent correction'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0457P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                2742
_reflns_number_total             4052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200414c.txt
_cod_data_source_block           compound_2
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-08-09
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7114381
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 '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
S1 S 0.65091(4) 0.98970(10) 0.72769(4) 0.03811(15) Uani 1 1 d
S2 S 0.60736(4) 1.40593(9) 0.57132(4) 0.03838(15) Uani 1 1 d
P P 0.68185(3) 1.14724(9) 0.60610(4) 0.02799(13) Uani 1 1 d
O O 1.08590(11) 1.3396(3) 0.63191(15) 0.0572(5) Uani 1 1 d
N1 N 0.67093(14) 0.9605(3) 0.51980(14) 0.0350(4) Uani 1 1 d
N2 N 0.54719(15) 1.1647(4) 0.36642(17) 0.0439(5) Uani 1 1 d
C1 C 0.69336(16) 0.9910(4) 0.41734(17) 0.0391(5) Uani 1 1 d
C2 C 0.60862(19) 0.9755(4) 0.35288(18) 0.0427(5) Uani 1 1 d
C3 C 0.80357(13) 1.2207(4) 0.61220(14) 0.0303(4) Uani 1 1 d
C4 C 0.86963(15) 1.0606(4) 0.59836(18) 0.0389(5) Uani 1 1 d
C5 C 0.96303(16) 1.1062(4) 0.60672(19) 0.0428(6) Uani 1 1 d
C6 C 0.99230(14) 1.3136(4) 0.62796(17) 0.0381(5) Uani 1 1 d
C7 C 0.92809(17) 1.4729(4) 0.6435(2) 0.0429(6) Uani 1 1 d
C8 C 0.83358(16) 1.4252(4) 0.63568(18) 0.0389(5) Uani 1 1 d
C9 C 1.1215(2) 1.5514(6) 0.6338(3) 0.0545(7) Uani 1 1 d
H1A H 0.7439(18) 0.887(5) 0.398(2) 0.058(8) Uiso 1 1 d
H1B H 0.7236(17) 1.129(4) 0.4078(18) 0.045(7) Uiso 1 1 d
HN1A H 0.6635(18) 0.847(4) 0.5376(19) 0.045(8) Uiso 1 1 d
H2 H 0.8514(15) 0.919(4) 0.5824(17) 0.038(6) Uiso 1 1 d
H2A H 0.5723(19) 0.867(4) 0.3722(19) 0.050(8) Uiso 1 1 d
HN2A H 0.569(2) 1.271(5) 0.331(2) 0.066(10) Uiso 1 1 d
HN2B H 0.479(2) 1.140(5) 0.352(2) 0.082(10) Uiso 1 1 d
H2B H 0.6308(17) 0.980(4) 0.2738(19) 0.049(7) Uiso 1 1 d
HN2C H 0.5417(18) 1.211(5) 0.433(2) 0.066(9) Uiso 1 1 d
H5 H 1.0084(18) 1.000(4) 0.6011(19) 0.055(8) Uiso 1 1 d
H7 H 0.9475(16) 1.596(4) 0.6525(18) 0.039(7) Uiso 1 1 d
H8 H 0.7948(16) 1.521(4) 0.6508(17) 0.033(6) Uiso 1 1 d
H9A H 1.102(2) 1.626(5) 0.581(3) 0.077(11) Uiso 1 1 d
H9B H 1.186(2) 1.541(5) 0.630(2) 0.061(8) Uiso 1 1 d
H9C H 1.101(3) 1.636(7) 0.689(3) 0.112(15) 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
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
N1 P C3 107.21(10)
N1 P S2 109.90(8)
C3 P S2 109.30(7)
N1 P S1 103.69(8)
C3 P S1 107.75(7)
S2 P S1 118.38(4)
C6 O C9 118.2(2)
C1 N1 P 125.25(17)
N1 C1 C2 112.1(2)
N2 C2 C1 111.0(2)
C8 C3 C4 118.3(2)
C8 C3 P 123.00(17)
C4 C3 P 118.57(17)
C5 C4 C3 120.8(2)
C4 C5 C6 120.3(2)
O C6 C7 125.4(2)
O C6 C5 114.9(2)
C7 C6 C5 119.7(2)
C6 C7 C8 119.6(2)
C3 C8 C7 121.2(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 P 1.9856(8)
S2 P 1.9850(8)
P N1 1.6625(19)
P C3 1.813(2)
O C6 1.359(3)
O C9 1.408(4)
N1 C1 1.457(3)
N2 C2 1.480(3)
C1 C2 1.508(3)
C3 C8 1.375(3)
C3 C4 1.388(3)
C4 C5 1.379(3)
C5 C6 1.382(3)
C6 C7 1.370(3)
C7 C8 1.397(3)
