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_4333531
_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 N3 Ni O2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C36.5 H56 Cl N3 Ni O2'
_chemical_formula_weight         663.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_audit_update_record
;
Collection: DBIMNI #7652
Collection strategy: HEMISPHERE, ??s frames, 0.3 degree \w scans.
Collected by: AJB
Processed by: AJB
Structure Solution by: MF (02/08/2010)
Structure Refinement by: MF (02/08/2010)
CIF checked (AJB/WL only): AJB (14/9/2010)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.265(3)
_cell_length_b                   27.289(5)
_cell_length_c                   13.671(2)
_cell_measurement_reflns_used    7914
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.504
_cell_volume                     7560(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_molecular_graphics    ' ?'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22558
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/2; Sheldrick, 2007)'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       column
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The electron count in the region of the diffuse solvent was 212 for
the unit cell, assigned as half a molecule of CH2Cl2 per asymmetric unit. 
The associated volume was 986 Angstrom**3 per unit cell.
;
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.27
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0435
_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^)+(0.078P)^2^+4.204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.125
_refine_ls_wR_factor_ref         0.130
_reflns_number_gt                3544
_reflns_number_total             4358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301731w_si_002_1.cif
_cod_data_source_block           dbimni
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4333531