[3,3',3''-(1,4,7-Triazacyclononane-1,4,7-triyl)tripropanamide]nickel(II) bis(perchlorate)
Liu, Rui; Li, Yi-Zhi; Zhang, Zhong; Wang, Zhi-Lin; Acta Crystallographica Section E 62 (2006) m1064–m1065; doi:10.1107/S1600536806013316

data_2208965
_publ_section_title
;
 [3,3',3''-(1,4,7-Triazacyclononane-1,4,7-triyl)tripropanamide]nickel(II)
 bis(perchlorate)
;
_journal_coeditor_code           OB2011
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1064
_journal_page_last               m1065
_journal_paper_doi               10.1107/S1600536806013316
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ni (C15 H30 N6 O3)] (Cl O4)2'
_chemical_formula_moiety         'C15 H30 N6 Ni O3 , 2(Cl O4)'
_chemical_formula_sum            'C15 H30 Cl2 N6 Ni O11'
_chemical_formula_weight         600.06
_chemical_name_systematic
;
[3,3',3''-(1,4,7-Triazacyclononane-1,4,7-triyl)tripropanamide]nickel(II)
bis(perchlorate)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 105.562(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.544(2)
_cell_length_b                   12.5781(14)
_cell_length_c                   10.7292(12)
_cell_measurement_reflns_used    1477
_cell_measurement_temperature    298
_cell_measurement_theta_max      20.74
_cell_measurement_theta_min      2.27
_cell_volume                     2410.8(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12942
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.403
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0553
_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^)+(0.07P)^2^+1.9365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                3802
_reflns_number_total             4726
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob2011.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2208965
_cod_database_fobs_code          2208965