Versatility of 2,6-diacetylpyridine (dap) hydrazones in stabilizing uncommon coordination geometries of Mn(II): synthesis, spectroscopic, magnetic and structural characterization.
Naskar, Subhendu; Mishra, Dipankar; Chattopadhyay, Shyamal Kumar; Corbella, Montserrat; Blake, Alexander J.; Dalton transactions (Cambridge, England : 2003)  (2005) 2428–2435; doi:10.1039/b503891j

data_7008526
_publ_section_title
;
 Versatility of 2,6-diacetylpyridine (dap) hydrazones in stabilizing
 uncommon coordination geometries of Mn(II): synthesis, spectroscopic,
 magnetic and structural characterization.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2428
_journal_page_last               2435
_journal_paper_doi               10.1039/b503891j
_journal_year                    2005
_chemical_formula_moiety         'C23 H23 Mn N5 O6, C3 H7 N O'
_chemical_formula_sum            'C26 H30 Mn N6 O7'
_chemical_formula_weight         593.50
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens
'water and Me H from delta-F; others geometrically placed'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.421(2)
_cell_angle_beta                 96.351(2)
_cell_angle_gamma                102.314(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4635(8)
_cell_length_b                   13.908(2)
_cell_length_c                   15.216(2)
_cell_measurement_reflns_used    5180
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     1369.5(3)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12210
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.9432
_exptl_absorpt_correction_T_min  0.8177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square tablet'
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.61
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment
'Water H with distance restraints; Me rigid rotating group; others riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5886
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.064P)^2^+0.075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.110
_reflns_number_gt                4794
_reflns_number_total             5886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503891j.txt
_cod_data_source_block           MNCOGE
_cod_original_cell_volume        1369.5(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008526