Bis[μ-<i>N</i>'-(adamantan-1-ylcarbonyl)-2-oxidobenzohydrazidato(3{-})]tetrapyridinetrinickel(II) dimethylformamide monosolvate monohydrate
Wei, Han-Chang; Huang, Wan-Yun; Zhou, Xiang; Shi, Meng; Liang, Fu-Pei; Acta Crystallographica Section E 68 (2012) m619–m620; doi:10.1107/S1600536812013396

data_2234840
_publ_section_title
;
 Bis[\m-<i>N</i>'-(adamantan-1-ylcarbonyl)-2-oxidobenzohydrazidato(3{-})]tetrapyridinetrinickel(II)
 dimethylformamide monosolvate monohydrate
;
_journal_coeditor_code           XU5481
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m619
_journal_page_last               m620
_journal_paper_doi               10.1107/S1600536812013396
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Ni3 (C18 H19 N2 O3)2 (C5 H5 N)4], C3 H7 N O, H2 O'
_chemical_formula_moiety         'C56 H58 N8 Ni3 O6, C3 H7 N O, H2 O'
_chemical_formula_sum            'C59 H67 N9 Ni3 O8'
_chemical_formula_weight         1206.35
_chemical_name_systematic
;
Bis[\m-<i>N</i>'-(adamantan-1-ylcarbonyl)-2-
oxidobenzohydrazidato(3-)]tetrapyridinetrinickel(II)
dimethylformamide monosolvate monohydrate
;
_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                62.0610(10)
_cell_angle_beta                 72.2610(10)
_cell_angle_gamma                85.2020(10)
_cell_formula_units_Z            2
_cell_length_a                   14.3496(8)
_cell_length_b                   14.8499(9)
_cell_length_c                   15.2256(9)
_cell_measurement_reflns_used    6088
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      26.0357
_cell_measurement_theta_min      2.2316
_cell_volume                     2723.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13829
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.8534
_exptl_absorpt_correction_T_min  0.7570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.657
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         9496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0519P)^2^+1.7341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                8034
_reflns_number_total             9496
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5481.cif
_cod_data_source_block           I
_cod_database_code               2234840
_cod_database_fobs_code          2234840