Bis[μ~2~-<i>N</i>'-acetyl-2-hydroxy-6-oxidobenzohydrazidato(3{-})]octapyridinetrinickel(II)
Yang, Yan; Li, Dacheng; Shi, Xuefeng; Acta Crystallographica Section E 65 (2009) m746–; doi:10.1107/S1600536809020534

data_2222281
_publ_section_title
Bis[\m~2~-<i>N</i>'-acetyl-2-hydroxy-6-oxidobenzohydrazidato(3{-})]octapyridinetrinickel(II)
_journal_coeditor_code           CV2565
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m746
_journal_paper_doi               10.1107/S1600536809020534
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni3 (C9 H7 N2 O4)2 (C5 H5 N)8]'
_chemical_formula_moiety         'C58 H54 N12 Ni3 O8'
_chemical_formula_sum            'C58 H54 N12 Ni3 O8'
_chemical_formula_weight         1223.26
_chemical_name_systematic
;
Bis[\m~2~-<i>N</i>'-acetyl-2-hydroxy-6-
oxidobenzohydrazidato(3-)]octapyridinetrinickel(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                 96.663(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9349(18)
_cell_length_b                   18.230(3)
_cell_length_c                   16.262(2)
_cell_measurement_reflns_used    4241
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.183
_cell_measurement_theta_min      2.235
_cell_volume                     2925.4(8)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.1464
_diffrn_reflns_av_sigmaI/netI    0.1418
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14103
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.6627
_exptl_absorpt_correction_T_min  0.6142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.44
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.577
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5138
_refine_ls_number_restraints     1098
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0747
_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^)+(0.0999P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.2100
_reflns_number_gt                3047
_reflns_number_total             5138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cv2565.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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        2925.3(8)
_cod_original_sg_symbol_H-M      'P 21/n  '
_cod_database_code               2222281
_cod_database_fobs_code          2222281