Aquabis(1,5-dimethyl-2-phenyl-4-{[(<i>E</i>)-4-pyridylmethylene-κ<i>N</i>]amino}pyrazolidin-3-one)dinitratonickel(II)
Hong Liang; Xian-Wen Wang; Zhen-Feng Chen; Ling Huang; Hong-Li Zou; Jian Zhou; Kai-Bei Yu; Acta Crystallographica Section E 60 (2004) m294–m296; doi:10.1107/S1600536804002636

data_2203345
_publ_section_title
Aquabis(1,5-dimethyl-2-phenyl-4-{[(<i>E</i>)-4-pyridylmethylene-\k<i>N</i>]amino}pyrazolidin-3-one)dinitratonickel(II)
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m294
_journal_page_last               m296
_journal_paper_doi               10.1107/S1600536804002636
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (N O3)2 (C17 H16 N4 O)2 (N O3)2 (H2 O)]'
_chemical_formula_moiety         'C34 H34 N10 Ni O9'
_chemical_formula_sum            'C34 H34 N10 Ni O9'
_chemical_formula_weight         785.42
_chemical_name_common
;
Dinitratoaquabis(3-pyrazolidinone,
1,5-dimethyl-2-phenyl-4-[{(E)-4-pyridinylmethylidene}amino])nickel(II)
;
_chemical_name_systematic
;
Aquabis(1,5-dimethyl-2-phenyl-4-{[(E)-4-pyridylmethylene-
\kN]amino}pyrazolidin-3-one)dinitratonickel(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.860(10)
_cell_angle_beta                 75.410(10)
_cell_angle_gamma                73.860(10)
_cell_formula_units_Z            2
_cell_length_a                   10.097(2)
_cell_length_b                   12.977(2)
_cell_length_c                   14.860(2)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.59
_cell_measurement_theta_min      2.83
_cell_volume                     1807.4(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'SXSCANS (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1997a)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7176
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        2.44
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.297
_refine_ls_extinction_coef       0.0020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6540
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0539P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                4930
_reflns_number_total             6540
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rn6009.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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_original_cell_volume        1807.3(5)
_cod_database_code               2203345
_cod_database_fobs_code          2203345