Stepwise Complexation of Ni(II) and Cu(II) Ions by 6,6'-C-spirobi(cyclam) (cyclam = 1,4,8,11-Tetraazacyclotetradecane), L1. Syntheses and Redox Chemistry of [M(H2L1)]X4 (M = Cu2+, Ni2+), [Cu2(L1)]X4, and [CuNi(L1)]X4 (X = ClO4-) and the X-ray Crystal Structure of [Cu2(L1)](ClO4)4
A. McAuley; M. J. Zaworotko; K. Biradha; Inorganic Chemistry 38 (1999) 5078–5085; doi:10.1021/ic9904844

data_4322352
_publ_section_title
;
 Stepwise Complexation of Ni(II) and Cu(II) Ions by 6,6'-C-spirobi(cyclam)
 (cyclam = 1,4,8,11-Tetraazacyclotetradecane), L1. Syntheses and Redox
 Chemistry of [M(H2L1)]X4 (M = Cu2+, Ni2+), [Cu2(L1)]X4, and [CuNi(L1)]X4
 (X = ClO4-) and the X-ray Crystal Structure of [Cu2(L1)](ClO4)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5078
_journal_page_last               5085
_journal_paper_doi               10.1021/ic9904844
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C19 H36 Cl4 Cu2 N8 O16'
_chemical_formula_weight         901.44
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                80.4450(10)
_cell_angle_beta                 76.1520(10)
_cell_angle_gamma                86.8760(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1143(5)
_cell_length_b                   12.6757(7)
_cell_length_c                   16.6980(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1644.21(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8734
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    1.702
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_F_000             920
_refine_diff_density_max         2.226
_refine_diff_density_min         -2.562
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.099
_refine_ls_goodness_of_fit_obs   1.185
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_restrained_S_obs      1.185
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_obs          0.1056
_refine_ls_shift/esd_max         -0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2122P)^2^+20.2914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3328
_refine_ls_wR_factor_obs         0.3200
_reflns_number_observed          4575
_reflns_number_total             5696
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9904844.cif
_cod_data_source_block           p1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2122P)^2^+20.2914P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2122P)^2^+20.2914P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1644.2(2)
_cod_database_code               4322352