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_7053835
_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         'C42 H68 N4 Ni O16 P2 S2'
_chemical_formula_sum            'C42 H68 N4 Ni O16 P2 S2'
_chemical_formula_weight         1069.77
_chemical_name_common
;Bis(N-diisopropoxy-N'-(benzo-15-crown-5-4'-yl)-thiocarbamido-
N,S)nickel
;
_chemical_name_systematic
Bis[N-diisopropoxy-N'-(benzo-15-crown-5-4'-yl)-thiocarbamido-N,S]nickel
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.214(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4922(15)
_cell_length_b                   15.482(3)
_cell_length_c                   32.203(6)
_cell_measurement_reflns_used    1554
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.98
_cell_measurement_theta_min      2.54
_cell_volume                     5222.8(16)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            5562
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              SmartApex2
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.8928
_exptl_absorpt_correction_T_min  0.8010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5266
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+4.6368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1403
_reflns_number_gt                3106
_reflns_number_total             5266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00252asup1.cif
_cod_data_source_block           z100
_cod_original_cell_volume        5222.8(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7053835