Structure of the adduct of bis(2,2'biimidazole)copper(II) perchlorate with 4,7-dihydro-1,2,4-triazolo[1,5-a]pyrimidine-7-one
Mohammad Abul-Haj; Miguel Quiros; Juan M. Salas; Journal of Chemical Crystallography 34 (2004) 549–552; doi:10.1023/B:JOCC.0000042024.70444.a0

data_1100152
_publ_section_title
;
 Structure of the adduct of bis(2,2'biimidazole)copper(II) perchlorate
 with 4,7-dihydro-1,2,4-triazolo[1,5-a]pyrimidine-7-one
;
_journal_issue                   8
_journal_name_full               'Journal of Chemical Crystallography'
_journal_page_first              549
_journal_page_last               552
_journal_paper_doi               10.1023/B:JOCC.0000042024.70444.a0
_journal_volume                  34
_journal_year                    2004
_chemical_formula_sum            'C22 H20 Cl2 Cu N16 O10'
_chemical_formula_weight         802.98
_chemical_name_systematic
'bis(2,2'-biimidazole)copper(II) perchlorate bis(4,7-dihydro-1,2,4-triazolo[1,5-a]pyrimidine-7-one'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 103.690(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.666(2)
_cell_length_b                   11.7586(8)
_cell_length_c                   13.4808(9)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      20.1
_cell_measurement_theta_min      12.5
_cell_volume                     3028.8(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 0.82 - 1.67, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4407
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        7.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.7873
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.16
    H   K   L   2Theta   Chi   Imin/Imax
    0   0   2     6.2    70.5    0.668
    0   0   4    12.5    70.5    0.775
   -5   1   6    19.6    75.4    0.822
   -2   2   7    22.4    75.8    0.824
   -6   2   7    23.7    71.5    0.803
   -2   0   8    24.4    79.5    0.822
    0   0   8    25.1    70.5    0.831
   -2   0  10    30.8    77.7    0.832
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.934
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0806
_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^)+(0.0950P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.2456
_reflns_number_gt                2586
_reflns_number_total             4407
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1100152