Tris(ethane-1,2-diamine-κ^2^<i>N</i>,<i>N</i>')nickel(II) 5-hydroxyisophthalate monohydrate
Wang, Shu-Hong; Zhang, Bin; Wang, Cheng; Xu, Guo-Qiang; Xie, Yang; Acta Crystallographica Section E 67 (2011) m257–m258; doi:10.1107/S1600536811001449

data_2229091
_publ_section_title
;
 Tris(ethane-1,2-diamine-\k^2^<i>N</i>,<i>N</i>')nickel(II)
 5-hydroxyisophthalate monohydrate
;
_journal_coeditor_code           HY2388
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m257
_journal_page_last               m258
_journal_paper_doi               10.1107/S1600536811001449
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni (C2 H8 N2)3] (C8 H4 O5), H2 O'
_chemical_formula_moiety         'C6 H24 N6 Ni 2+, C8 H4 O5 2-, H2 O'
_chemical_formula_sum            'C14 H30 N6 Ni O6'
_chemical_formula_weight         437.13
_chemical_name_systematic
;
Tris(ethane-1,2-diamine-\k^2^<i>N</i>,<i>N</i>')nickel(II) 5-hydroxyisophthalate
monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.000
_cell_angle_beta                 97.747(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   8.208(5)
_cell_length_b                   14.590(5)
_cell_length_c                   16.581(5)
_cell_measurement_reflns_used    3656
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.00
_cell_measurement_theta_min      2.00
_cell_volume                     1967.5(15)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8306
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3656
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.2444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                2997
_reflns_number_total             3656
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2388.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229091
_cod_database_fobs_code          2229091