Bis(4-acetyl-3-methyl-1-phenyl-1<i>H</i>-pyrazol-5-olato-κ^2^<i>O</i>,<i>O</i>')bis(<i>N</i>,<i>N</i>-dimethylformamide-κ<i>O</i>)nickel(II)
Zhu, Hualing; Wei, Zhen; Bu, Luxia; Xu, Xiaoping; Shi, Jun; Acta Crystallographica Section E 66 (2010) m904–; doi:10.1107/S1600536810026231

data_2226988
_publ_section_title
;
 Bis(4-acetyl-3-methyl-1-phenyl-1<i>H</i>-pyrazol-5-olato-\k^2^<i>O</i>,<i>O</i>')bis(<i>N</i>,<i>N</i>-dimethylformamide-\k<i>O</i>)nickel(II)
;
_journal_coeditor_code           LH5075
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m904
_journal_paper_doi               10.1107/S1600536810026231
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (C12 H11 N2 O2)2 (C3 H7 N O)2]'
_chemical_formula_moiety         'C30 H36 N6 Ni O6'
_chemical_formula_sum            'C30 H36 N6 Ni O6'
_chemical_formula_weight         635.36
_chemical_name_systematic
;
Bis(4-acetyl-3-methyl-1-phenyl-1<i>H</i>-pyrazol-5-olato-
\k^2^<i>O</i>,<i>O</i>')bis(<i>N</i>,<i>N</i>-dimethylformamide-
\k<i>O</i>)nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7201(17)
_cell_length_b                   17.119(3)
_cell_length_c                   9.852(2)
_cell_measurement_reflns_used    4482
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      2.384
_cell_volume                     1440.9(5)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10320
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.9307
_exptl_absorpt_correction_T_min  0.8680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Crystalclear; Rigaku, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.584
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0480P)^2^+0.3836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                2279
_reflns_number_total             2529
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5075.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2226988
_cod_database_fobs_code          2226988