The influence of the intramolecular hydrogen bond on the 1,3-N,S- and 1,5-O,S-coordination of N-phosphoryl-N′-(R)-thioureas with Ni(ii) and Pd(ii)
Sokolov, Felix D.; Baranov, Sergey V.; Safin, Damir A.; Hahn, F. Ekkehardt; Kubiak, Maria; Pape, Tania; Babashkina, Maria G.; Zabirov, Nail G.; Galezowska, Joanna; Kozlowski, Henryk; Cherkasov, Rafael A.; New Journal of Chemistry 31 (2007) 1661–; doi:10.1039/b702896b

data_7052184
_publ_section_title
;
 The influence of the intramolecular hydrogen bond on the 1,3-N,S- and
 1,5-O,S-coordination of N-phosphoryl-N&#x2032;-(R)-thioureas with
 Ni(ii) and Pd(ii)
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1661
_journal_paper_doi               10.1039/b702896b
_journal_volume                  31
_journal_year                    2007
_chemical_formula_sum            'C14 H44 N4 Ni O8 P2 S2'
_chemical_formula_weight         749.44
_chemical_name_common
;Bis(N-(diisopropoxyphosphoryl)-N'-(p-metoxyphenyl)
thiocarbamido-N,S)nickel(ii)
;
_chemical_name_systematic
;
Bis[N-(diisopropoxyphosphoryl)-N'-(p-metoxyphenyl)
thiocarbamido-N,S]nickel(II)
;
_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                 91.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.194(2)
_cell_length_b                   8.439(2)
_cell_length_c                   16.951(3)
_cell_measurement_reflns_used    2031
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      3.16
_cell_volume                     1743.7(6)
_computing_cell_refinement
'KM4 CCD Software (Oxford Diffraction Poland Sp, (1995-2005)'
_computing_data_collection
'KM4 CCD Software (Oxford Diffraction Poland Sp, (1995-2005)'
_computing_data_reduction
'KM4 CCD Software (Oxford Diffraction Poland Sp, (1995-2005)'
_computing_molecular_graphics    'ORTEP III Farrugia 1997'
_computing_publication_material  'SHELXL-97 Sheldrick 1997'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'KM4 CCD'
_diffrn_measurement_method       '/w 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  0.0950
_diffrn_reflns_av_sigmaI/netI    0.1914
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12428
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                2081
_reflns_number_total             4044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702896b.txt
_cod_data_source_block           kaz78abs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7052184