(μ~3~-Benzene-1,3,5-tricarboxylato)tris[aqua(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''-pentamethyldiethylenetriamine)nickel(II)] tris(perchlorate) 4.25-hydrate
Trávníček, Zdeněk; Marek, Jaromír; Čermáková, Šárka; Acta Crystallographica Section E 63 (2007) m2860–m2861; doi:10.1107/S1600536807051938

data_2216149
_publ_section_title
;(\m~3~-Benzene-1,3,5-tricarboxylato)tris[aqua(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''-pentamethyldiethylenetriamine)nickel(II)]
 tris(perchlorate) 4.25-hydrate
;
_journal_coeditor_code           TK2201
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2860
_journal_page_last               m2861
_journal_paper_doi               10.1107/S1600536807051938
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[Ni3 (C9 H3 O6) (C9 H23 N3)3 (H2 O)3] (Cl O4)3, 4.25H2 O'
_chemical_formula_moiety         'C36 H78 N9 Ni3 O9 3+, 3(Cl O4 -), 4.25(H2 O)'
_chemical_formula_sum            'C36 H86.5 Cl3 N9 Ni3 O25.25'
_chemical_formula_weight         1332.12
_chemical_name_systematic
;
(\m~3~-Benzene-1,3,5-tricarboxylato)tris[aqua(<i>N</i>,<i>N</i>,N',N'',N''-
pentamethyldiethylenetriamine)nickel(II)] tris(perchlorate) 4.25-hydrate
;
_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
_cell_angle_beta                 107.633(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7409(2)
_cell_length_b                   30.6727(5)
_cell_length_c                   16.9590(4)
_cell_measurement_reflns_used    25991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.6
_cell_volume                     5820.4(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3611
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2 + CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27090
_diffrn_reflns_theta_full        25.1
_diffrn_reflns_theta_max         25.1
_diffrn_reflns_theta_min         2.6
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2810
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.01
_refine_diff_density_min         -1.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         10209
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.03P)^2^+15P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.090
_refine_ls_wR_factor_ref         0.096
_reflns_number_gt                8075
_reflns_number_total             10209
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk2201.cif
_cod_data_source_block           I
_cod_original_cell_volume        5820.41(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C36 H86.50 Cl3 N9 Ni3 O25.25'
_cod_database_code               2216149
_cod_database_fobs_code          2216149