(3-Acetyl-4-methyl-1<i>H</i>-pyrazol-1-ide-5-carboxylato)bis(1,10-phenanthroline)nickel(II) 3.5-hydrate
Malinkin, Sergey; Kapshuk, Anatoliy A.; Gumienna-Kontecka, Elzbieta; Prisyazhnaya, Elena V.; Iskenderov, Turganbay S.; Acta Crystallographica Section E 69 (2013) m417–m418; doi:10.1107/S1600536813017194

data_2238253
_publ_section_title
;
 (3-Acetyl-4-methyl-1<i>H</i>-pyrazol-1-ide-5-carboxylato)bis(1,10-phenanthroline)nickel(II)
 3.5-hydrate
;
_journal_coeditor_code           SJ5334
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m417
_journal_page_last               m418
_journal_paper_doi               10.1107/S1600536813017194
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ni (C7 H6 N2 O3) (C12 H8 N2)2] , 3.5H2 O'
_chemical_formula_moiety         'C31 H22 N6 Ni O3, 3.5(H2 O)'
_chemical_formula_sum            'C31 H29 N6 Ni O6.5'
_chemical_formula_weight         648.29
_chemical_name_systematic
'(3-Acetyl-4-methyl-1<i>H</i>-pyrazol-1-ide-5-carboxylato)bis(1,10-phenanthroline)nickel(II) 3.5-hydrate'
_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           SHELXL97
_cell_angle_alpha                91.91(3)
_cell_angle_beta                 98.85(3)
_cell_angle_gamma                105.20(4)
_cell_formula_units_Z            2
_cell_length_a                   9.865(3)
_cell_length_b                   11.659(4)
_cell_length_c                   13.561(5)
_cell_measurement_reflns_used    11133
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      36.4590
_cell_measurement_theta_min      3.4140
_cell_volume                     1482.8(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'WinGX (Farrugia, 2012)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_sigmaI/netI    0.1791
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12624
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.55
_diffrn_reflns_theta_min         2.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9287
_exptl_absorpt_correction_T_min  0.8569
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.588
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6830
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                3040
_reflns_number_total             6830
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5334.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C31 H29 N6 Ni1 O6.5'
_cod_database_code               2238253
_cod_database_fobs_code          2238253