Crystal structure, supramolecular assembly and preliminary reactivity behaviour of new heteropolytopic ligands based on oxalate/malonate skeleton and azolate moieties
Garau, Federica; Monari, Magda; Pandolfo, Luciano; Pettinari, Claudio; Venzo, Alfonso; CrystEngComm 12 (2010) 1217–; doi:10.1039/b922874h

data_7212223
_publ_section_title
;
 Crystal structure, supramolecular assembly and preliminary reactivity
 behaviour of new heteropolytopic ligands based on oxalate/malonate
 skeleton and azolate moieties
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              1217
_journal_paper_doi               10.1039/b922874h
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C16 H10 N4 O2'
_chemical_formula_weight         290.28
_space_group_IT_number           2
_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                75.374(2)
_cell_angle_beta                 83.368(2)
_cell_angle_gamma                79.040(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3930(10)
_cell_length_b                   7.6748(11)
_cell_length_c                   12.1165(17)
_cell_measurement_temperature    296(2)
_cell_volume                     651.43(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5408
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.102
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             300
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0556P)^2^+0.1821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                2599
_reflns_number_total             2908
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b922874h.txt
_cod_data_source_block           ind_0m
_cod_database_code               7212223