Nickel(II) Complexes of Monofunctionalized Pyridine-Azamacrocycles: Synthesis, Structures, Pendant Arm "On-Off" Coordination Equilibria, and Peroxidase-like Activity
Voltaire G. Organo; Alexander S. Filatov; Justin S. Quartararo; Zachary M. Friedman; Elena V. Rybak-Akimova; Inorganic Chemistry 48 (2009) 8456–8468; doi:10.1021/ic901083u

data_4303098
_publ_contact_author_address
;
Department of Chemistry
Tufts University
Medford MA 02155
USA
;
_publ_contact_author_email       erybakak@granite.tufts.edu
_publ_contact_author_fax         617-627-3443
_publ_contact_author_name
;
Rybak-Akimova, Elena V. 
;
_publ_contact_author_phone       617-627-3413
_publ_section_title
;
Nickel(II) Complexes of Monofunctionalized Pyridine-Azamacrocycles:
Synthesis, Structures, Pendant Arm "On-Off" Coordination Equilibria,
and Peroxidase-like Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8456
_journal_page_last               8468
_journal_paper_doi               10.1021/ic901083u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C18 H30 N4 Ni O2, 2(Cl O4), H2 O'
_chemical_formula_sum            'C18 H32 Cl2 N4 Ni O11'
_chemical_formula_weight         610.09
_chemical_name_systematic
; 
 (3-[(2R,12S)-2,12-dimethyl-3,7,11,17-tetrazabicyclo[11.3.1]heptadeca-
1(16),13(17),14-trien-7-yl]propanoic acid)-nickel(II) diperchlorate monohydrate 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.136(2)
_cell_angle_beta                 81.401(2)
_cell_angle_gamma                70.847(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3224(11)
_cell_length_b                   11.7217(14)
_cell_length_c                   12.2905(15)
_cell_measurement_reflns_used    4595
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.24
_cell_volume                     1217.7(3)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30\% \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10708
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_correction_T_min  0.8545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0870P)^2^+0.3870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1567
_reflns_number_gt                4149
_reflns_number_total             5478
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic901083u_si_001_5.cif
_cod_data_source_block           '[Ni(LCOOH)](ClO4)2'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_Hall     '-P 1        '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4303098