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_4333534
_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         'C37 H57 N3 Ni O2, B F4'
_chemical_formula_sum            'C37 H57 B F4 N3 Ni O2'
_chemical_formula_weight         721.38
_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                 114.466(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7143(6)
_cell_length_b                   10.7572(2)
_cell_length_c                   19.8843(6)
_cell_measurement_reflns_used    6937
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.41
_cell_measurement_theta_min      4.11
_cell_volume                     3643.54(19)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    ' ? '
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13817
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.59
_diffrn_reflns_theta_min         4.24
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.1612
_exptl_crystal_size_mid          0.1070
_exptl_crystal_size_min          0.0717
_refine_diff_density_max         1.26
_refine_diff_density_min         -0.73
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7137
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+3.7501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                6123
_reflns_number_total             7137
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301731w_si_002_4.cif
_cod_data_source_block           nimflq
_cod_original_cell_volume        3643.53(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4333534
_nottingham_internal_coll_name   NIMFLQ
_nottingham_internal_coll_number 9950
_nottingham_internal_coll_client MF/JM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '11 and 44s'
_nottingham_internal_coll_frame_width '1 degree'
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   wl
_nottingham_internal_coll_date   5/1/2011
_nottingham_internal_process_user wl
_nottingham_internal_process_date 05/01/2011
_nottingham_internal_solution_user mf
_nottingham_internal_solution_date 05/01/2011
_nottingham_internal_refinement_user mf
_nottingham_internal_refinement_date 05/01/2011
_nottingham_internal_validation_user wl
_nottingham_internal_validation_date 1/3/2011
_nottingham_internal_archive_date 1/3/2011