Aquadipyridinebis(<i>N</i>-<i>p</i>-tolysulfonyl-<small>L</small>-leucinato)nickel(II)
Tai, Xi-Shi; Acta Crystallographica Section E 66 (2010) m1346–; doi:10.1107/S1600536810038493

data_2227536
_publ_section_title
;
 Aquadipyridinebis(<i>N</i>-<i>p</i>-tolysulfonyl-<small>L</small>-leucinato)nickel(II)
;
_journal_coeditor_code           HB5641
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1346
_journal_paper_doi               10.1107/S1600536810038493
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C13 H18 N O4 S)2 (C5 H5 N)2 (H2 O)]'
_chemical_formula_moiety         'C36 H48 N4 Ni O9 S2'
_chemical_formula_sum            'C36 H48 N4 Ni O9 S2'
_chemical_formula_weight         803.61
_chemical_name_systematic
;
Aquadipyridinebis(<i>N</i>-<i>p</i>-tolysulfonyl-L-leucinato)nickel(II)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.1023(16)
_cell_length_b                   19.5538(19)
_cell_length_c                   22.956(2)
_cell_measurement_reflns_used    6010
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.567
_cell_measurement_theta_min      2.368
_cell_volume                     8125.7(13)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41421
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.8275
_exptl_absorpt_correction_T_min  0.7944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.732
_refine_ls_abs_structure_details 'Flack (1983), <b>6501 Friedel pairs</b>'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         14319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1133P)^2^+9.1777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.2415
_reflns_number_gt                8009
_reflns_number_total             14319
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hb5641.cif
_cod_data_source_block           I
_cod_database_code               2227536
_cod_database_fobs_code          2227536