μ-Oxalato-bis[(1,4,8,11-tetraazacyclotetradecane)nickel(II)] bis(perchlorate) hemihydrate
Hui Liu; Wu Gu; Xiao-Lan Tong; Ying-Ying Kou; Shi-Ping Yan; Acta Crystallographica Section E 62 (2006) m2704–m2705; doi:10.1107/S1600536806037901

data_2210507
_publ_section_title
;
 \m-Oxalato-bis[(1,4,8,11-tetraazacyclotetradecane)nickel(II)]
 bis(perchlorate) hemihydrate
;
_journal_coeditor_code           BI2062
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2704
_journal_page_last               m2705
_journal_paper_doi               10.1107/S1600536806037901
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ni2 (C2 O4) (C20 H48 N8] (Cl O4)2, 0.5H2 O'
_chemical_formula_moiety         'C22 H48 N8 Ni2 O4 2+, 2Cl O4 -, 0.5H2 O'
_chemical_formula_sum            'C22 H49 Cl2 N8 Ni2 O12.5'
_chemical_formula_weight         814.01
_chemical_name_systematic
;\m-Oxalato-bis[(1,4,8,11-tetraazacyclotetradecane)nickel(II)]
 bis(perchlorate)
hemihydrate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 104.513(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.854(2)
_cell_length_b                   13.350(3)
_cell_length_c                   15.245(4)
_cell_measurement_reflns_used    2035
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.35
_cell_measurement_theta_min      2.43
_cell_volume                     1744.5(7)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8405
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.361
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3067
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.2902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1283
_reflns_number_gt                1951
_reflns_number_total             3067
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2062.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2210507
_cod_database_fobs_code          2210507