A binuclear unsymmetrical compartmental Ni^II^ complex: [μ-11,24-dimethyl-16,19-dioxa-3,7,15,20-tetraazatricyclo[20.3.1.1^9,13^]heptacosa-1(25),2,7,9,11,13(27),14,20,22(26),23-decaene-26,27-diolato]bis[diaquanickel(II)] bis(perchlorate) tetrahydrate
S. Anbu; M. Kandaswamy; Babu Varghese; Acta Crystallographica Section E 63 (2007) m2330–m2331; doi:10.1107/S1600536807039001

data_2215048
_publ_section_title
;A binuclear unsymmetrical compartmental Ni^II^ complex:
 [\m-11,24-dimethyl-16,19-dioxa-3,7,15,20-tetraazatricyclo[20.3.1.1^9,13^]heptacosa-1(25),2,7,9,11,13(27),14,20,22(26),23-decaene-26,27-diolato]bis[diaquanickel(II)]
 bis(perchlorate) tetrahydrate
;
_journal_coeditor_code           CI2420
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2330
_journal_page_last               m2331
_journal_paper_doi               10.1107/S1600536807039001
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni2 (C23 H24 N4 O4) (H2 O)4] (Cl O4)2, 4H2 O'
_chemical_formula_moiety         'C23 H32 N4 Ni2 O8, 2(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C23 H40 Cl2 N4 Ni2 O20'
_chemical_formula_weight         880.91
_chemical_name_systematic
;
[\m-11,24-dimethyl-16,19-dioxa-3,7,15,20-
tetraazatricyclo[20.3.1.1^9,13^]heptacosa-
1(25),2,7,9,11,13(27),14,20,22(26),23-decaene-26,27-
diolato]bis[diaquanickel(II)] bis(perchlorate) tetrahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                107.167(2)
_cell_angle_beta                 94.932(2)
_cell_angle_gamma                103.092(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5227(3)
_cell_length_b                   10.3081(3)
_cell_length_c                   12.2764(5)
_cell_measurement_reflns_used    7997
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.5
_cell_measurement_theta_min      2.2
_cell_volume                     873.89(6)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.790
_diffrn_measurement_device_type  'Bruker Kappa-APEXII area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24651
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         37.33
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  0.8254
_exptl_absorpt_correction_T_min  0.7321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         7176
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0342
_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^)+(0.067P)^2^+0.1283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                5831
_reflns_number_total             7176
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2420.cif
_cod_data_source_block           I
_cod_database_code               2215048
_cod_database_fobs_code          2215048