Syntheses, crystal structures and magnetic properties of new oxalato-, croconato- and squarato-containing copper(II) complexes
José Carranza; Conor Brennan; Jorunn Sletten; Brita Vangdal; Paul Rillema; Francesc Lloret; Miguel Julve; New J. Chem. 27 (2003) 1775–1783; doi:10.1039/b301212n

data_7050560
_publ_section_title
;
 Syntheses, crystal structures and magnetic properties of new oxalato-,
 croconato- and squarato-containing copper(II) complexes
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1775
_journal_page_last               1783
_journal_paper_doi               10.1039/b301212n
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C13 H8 Cu N4 O6'
_chemical_formula_weight         379.77
_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 if bound to C, difmap if bound to O'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.3160(10)
_cell_angle_beta                 97.9950(10)
_cell_angle_gamma                107.8400(10)
_cell_formula_units_Z            2
_cell_length_a                   6.7113(4)
_cell_length_b                   9.2977(5)
_cell_length_c                   11.8250(6)
_cell_measurement_reflns_used    4899
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.9
_cell_measurement_theta_min      2.5
_cell_volume                     653.32(6)
_computing_cell_refinement       'SAINT, version 6.02a'
_computing_data_collection       'SMART, version 5.054'
_computing_data_reduction        'SAINT, version 6.02a'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  '2K SMART CCD'
_diffrn_measurement_method       'omega scan'
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6057
_diffrn_reflns_theta_full        32.09
_diffrn_reflns_theta_max         32.09
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_number
'50 first frames remeasured at end of experiment'
_exptl_absorpt_coefficient_mu    1.717
_exptl_absorpt_correction_T_max  'see above'
_exptl_absorpt_correction_T_min  'Tmin/Tmax ratio 0.768846'
_exptl_absorpt_correction_type   'empirical, SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0418P)^2^+0.2473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                3684
_reflns_number_total             4055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301212n.txt
_cod_data_source_block           13jc
_cod_original_cell_volume        653.31(6)
_cod_database_code               7050560