Aqua(pyridine <i>N</i>-oxide-κ<i>O</i>)[tris(2-hydroxyaminopropyl)amine-κ^4^<i>N</i>]nickel(II) dinitrate
Edison, Sara E.; Krause Bauer, Jeanette A.; Baldwin, Michael J.; Acta Crystallographica Section E 60 (2004) m1930–m1932; doi:10.1107/S160053680403003X

data_2204748
_publ_section_title
;Aqua(pyridine
 <i>N</i>-oxide-\k<i>O</i>)[tris(2-hydroxyaminopropyl)amine-\k^4^<i>N</i>]nickel(II)
 dinitrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1930
_journal_page_last               m1932
_journal_paper_doi               10.1107/S160053680403003X
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'[Ni (C5 H5 N O) (C9 H18 N4 O3) (H2 O)] (N O3)2'
_chemical_formula_moiety         'C14 H25 N5 Ni O5 2+, 2N O3 -'
_chemical_formula_sum            'C14 H25 N7 Ni O11'
_chemical_formula_weight         526.12
_chemical_name_systematic
;
Aqua(pyridine N-oxide-\kO)[tris(2-hydroxyaminopropyl)amine-\k^4^N]nickel(II)
dinitrate
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   mixed
_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            4
_cell_length_a                   11.0671(10)
_cell_length_b                   14.0481(10)
_cell_length_c                   14.8625(12)
_cell_measurement_reflns_used    5192
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      29.40
_cell_measurement_theta_min      2.71
_cell_volume                     2310.7(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7484
_diffrn_reflns_theta_full        29.40
_diffrn_reflns_theta_max         29.40
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.487
_refine_ls_abs_structure_details 'Flack (1983), 1736 Friedel pairs'
_refine_ls_abs_structure_Flack   0.065(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0328P)^2^+1.1661P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                2427
_reflns_number_total             2547
_reflns_threshold_expression     I>2\s(I)'
_cod_data_source_file            lh6317.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2204748
_cod_database_fobs_code          2204748