Synthesis and hydrolysis of cis-octahedral nickel(II) complexes with C-racemic tetraaza macrocycles bearing two imidate ester pendant arms
Soonmoo Bang; Nahee Kim; Shin-Geol Kang; Jong Hwa Jeong; Inorganica Chimica Acta 392 (2012) 184–191; doi:10.1016/j.ica.2012.05.035

data_1512480
_publ_section_title
;
 Synthesis and hydrolysis of cis-octahedral nickel(II) complexes with
 C-racemic tetraaza macrocycles bearing two imidate ester pendant arms
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              184
_journal_page_last               191
_journal_paper_doi               10.1016/j.ica.2012.05.035
_journal_volume                  392
_journal_year                    2012
_chemical_formula_moiety         'C22 H46 N6 Ni O2, C2 H3 N, 2(Cl O4)'
_chemical_formula_sum            'C24 H49 Cl2 N7 Ni O10'
_chemical_formula_weight         725.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.251(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8688(14)
_cell_length_b                   17.306(2)
_cell_length_c                   15.1606(17)
_cell_measurement_reflns_used    7357
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.27
_cell_volume                     3341.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_sigmaI/netI    0.1068
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24487
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0766
_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^)+(0.1362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2763
_reflns_number_gt                4544
_reflns_number_total             8268
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-184-191-2.cif
_cod_data_source_block           KANG11j
_cod_original_cell_volume        3341.5(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1512480