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_4303094
_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         'C20 H34 N6 Ni O, C2 H3 N, 2(Cl O4)'
_chemical_formula_sum            'C22 H37 Cl2 N7 Ni O9'
_chemical_formula_weight         673.20
_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]propanamide)-acetonitrile-nickel(II) 
diperchlorate acetonitrile solvate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 108.913(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2106(15)
_cell_length_b                   14.6125(17)
_cell_length_c                   16.2692(19)
_cell_measurement_reflns_used    5882
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.62
_cell_volume                     2971.0(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.944
_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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25486
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.8777
_exptl_absorpt_correction_T_min  0.8558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0722P)^2^+3.8665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                5529
_reflns_number_total             6971
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic901083u_si_001_1.cif
_cod_data_source_block           '[Ni(LCONH2)](ClO4)2*CH3CN'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 2ybc     '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4303094