Five Coordinate M(II)-Diphenolate [M = Zn(II), Ni(II), and Cu(II)] Schiff Base Complexes Exhibiting Metal- and Ligand-Based Redox Chemistry
Mark Franks; Anastasia Gadzhieva; Laura Ghandhi; David Murrell; Alexander J. Blake; E. Stephen Davies; William Lewis; Fabrizio Moro; Jonathan McMaster; Martin Schröder; Inorganic Chemistry 52 (2013) 660–670; doi:10.1021/ic301731w

data_4333537
_publ_contact_author_address
;
  School of Chemistry
  The University of Nottingham
  University Park
  Nottingham  NG7 2RD
  England UK
;
_publ_contact_author_email       j.mcmaster@nottingham.ac.uk
_publ_contact_author_fax         '0115 951 3563'
_publ_contact_author_name        'Dr Jonathan McMaster'
_publ_contact_author_phone       '0115 951 3498'
_publ_section_title
;
 Five Coordinate M(II)-Diphenolate [M = Zn(II), Ni(II), and Cu(II)] Schiff
 Base Complexes Exhibiting Metal- and Ligand-Based Redox Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              660
_journal_page_last               670
_journal_paper_doi               10.1021/ic301731w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C36 H55 Cu N3 O2, 0.25(C H4 O)'
_chemical_formula_sum            'C36.25 H56 Cu N3 O2.25'
_chemical_formula_weight         633.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   26.0367(17)
_cell_length_b                   26.0367(17)
_cell_length_c                   20.857(3)
_cell_measurement_reflns_used    43969
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21.48
_cell_measurement_theta_min      2.24
_cell_volume                     14139(2)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35499
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             5464
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
Approximately 3.1% of the unit cell volume comprises
a region of disordered solvent which could not be 
modelled as discrete atomic sites.  We employed PLATON 
SQUEEZE to calculate the solvent contribution to the 
diffraction.  SQUEEZE estimated a total of 79.2 electrons
per unit cell associated with FOUR molecules of 
CH3OH, and thereby produced a set of solvent-free
diffraction intensities.
;
_refine_diff_density_max         0.80
_refine_diff_density_min         -0.43
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6219
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0522P)^2^+41.7977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                4769
_reflns_number_total             6219
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301731w_si_002_7.cif
_cod_data_source_block           cumfld
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4333537
_nottingham_internal_coll_name   CUMFLD
_nottingham_internal_coll_number 9691
_nottingham_internal_coll_client MF/JM
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_frame_time '10 s'
_nottingham_internal_coll_frame_width '0.3 degrees'
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   MF
_nottingham_internal_coll_date   31/08/2010
_nottingham_internal_process_user MF
_nottingham_internal_process_date 31/08/2010
_nottingham_internal_solution_user MF
_nottingham_internal_solution_date 1/09/2010
_nottingham_internal_refinement_user MF
_nottingham_internal_refinement_date 1/09/2010
_nottingham_internal_validation_user WL
_nottingham_internal_validation_date 28/2/2011
_nottingham_internal_archive_date 28/2/2011