Tris(1,3-diaminopropane-<i>N</i>,<i>N</i>')nickel(II) diperchlorate
Olof Kristiansson; Acta Crystallographica Section C 55 (1999) IUC9900038–; doi:10.1107/S0108270199099539

data_2008493
_publ_section_title
;
 Tris(1,3-diaminopropane-<i>N</i>,<i>N</i>')nickel(II) diperchlorate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900038
_journal_paper_doi               10.1107/S0108270199099539
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Ni (C3 H10 N2)3] (Cl1 O4)2'
_chemical_formula_moiety         'C9 H30 Cl2 N6 Ni1 O8'
_chemical_formula_sum            'C9 H30 Cl2 N6 Ni O8'
_chemical_formula_weight         480.00
_chemical_name_common
;
Tris(1,3-diaminopropane-N,N')nickel(II) diperchlorate
;
_chemical_name_systematic
;
Tris(1,3-diaminopropane-N,N')nickel(II) diperchlorate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   14.0600(9)
_cell_length_b                   26.4879(16)
_cell_length_c                   32.732(2)
_cell_measurement_reflns_used    8985
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      1.24
_cell_volume                     12190.0(13)
_computing_cell_refinement       'SMART and SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.039
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            70811
_diffrn_reflns_theta_full        28.59
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%
;
Neglible as determined from a repetition of the first 50 frames
at the end of the experiment
;
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6048
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.952
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         14633
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.104
_refine_ls_R_factor_gt           0.060
_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^)+(0.1103P)^2^+7.1536P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.195
_reflns_number_gt                8964
_reflns_number_total             14633
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qa0097.cif
_cod_data_source_block           QA0097
_cod_database_code               2008493