Predictable and unpredictable reactions between 4,4′-dipyridyldisulfide and phosphonodithioato/dithiophosphato NiII complexes: novel coordination polymers and the unique example of 4,4′-dipyridyltrisulfide
Aragoni, M. Carla; Arca, Massimiliano; Crespo, Miriam; Devillanova, Francesco A.; Hursthouse, Michael B.; Huth, Susanne L.; Isaia, Francesco; Lippolis, Vito; Verani, Gaetano; CrystEngComm 9 (2007) 873–; doi:10.1039/b708972d

data_7203048
_publ_section_title
;
 Predictable and unpredictable reactions between
 4,4&#x2032;-dipyridyldisulfide and phosphonodithioato/dithiophosphato
 NiII complexes: novel coordination polymers and the unique example of
 4,4&#x2032;-dipyridyltrisulfide
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              873
_journal_paper_doi               10.1039/b708972d
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C18 H28 N2 Ni O4 P2 S5'
_chemical_formula_weight         617.37
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.453(7)
_cell_angle_beta                 99.986(5)
_cell_angle_gamma                94.511(9)
_cell_formula_units_Z            2
_cell_length_a                   8.1601(4)
_cell_length_b                   9.4126(11)
_cell_length_c                   17.9991(9)
_cell_measurement_reflns_used    6130
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1334.85(19)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick ,1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\F & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49804
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.8839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.766
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         6113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0393
_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/[\s^2^(Fo^2^)+(0.0680P)^2^+1.8065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                5918
_reflns_number_total             6113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708972d.txt
_cod_data_source_block           04slh0874
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        1334.85(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7203048