The influence of an intramolecular hydrogen bond on the 1,3-N,S-coordination of crown ether-containing N-phosphorylthiourea with NiII
Safin, Damir A.; Babashkina, Maria G.; Klein, Axel; Sokolov, Felix D.; Baranov, Sergey V.; Pape, Tania; Hahn, F. Ekkehardt; Krivolapov, Dmitriy B.; New Journal of Chemistry 33 (2009) 2443–; doi:10.1039/b9nj00252a

data_7053834
_publ_section_title
;
 The influence of an intramolecular hydrogen bond on the
 1,3-N,S-coordination of crown ether-containing N-phosphorylthiourea with
 NiII
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2443
_journal_paper_doi               10.1039/b9nj00252a
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C21 H35 N2 O8 P S'
_chemical_formula_sum            'C21 H35 N2 O8 P S'
_chemical_formula_weight         506.54
_chemical_name_common
N-diisopropoxyphosphinyl-N'-(benzo-15-crown-5)-4'-yl-thiourea
_chemical_name_systematic
'N-diisopropoxyphosphinyl-N'-(benzo-15-crown-5)-4'-yl-thiourea '
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 106.486(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.721(19)
_cell_length_b                   8.715(5)
_cell_length_c                   9.919(6)
_cell_measurement_reflns_used    2747
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.21
_cell_measurement_theta_min      2.68
_cell_volume                     2629(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7658
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.43
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              SmartApex2
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.9557
_exptl_absorpt_correction_T_min  0.9557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4826
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                3430
_reflns_number_total             4826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00252asup1.cif
_cod_data_source_block           s7
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7053834