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_7050559
_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            'C8 H10 Cu N4 O6'
_chemical_formula_weight         321.74
_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 or N, difmap if bound to O'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.2660(10)
_cell_angle_beta                 106.7790(10)
_cell_angle_gamma                103.5270(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9893(4)
_cell_length_b                   9.2227(5)
_cell_length_c                   9.8112(5)
_cell_measurement_reflns_used    3274
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2.4
_cell_volume                     561.45(5)
_computing_cell_refinement       'SAINT, version 6.02A'
_computing_data_collection       'SMART, version 5.054'
_computing_data_reduction        'SAINT, version 6.02A'
_computing_molecular_graphics    'XP, version 5.1'
_computing_publication_material  'XCIF, version 5.10'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4689
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        1
_diffrn_standards_number
'50 first frames remeasured at end of experiment'
_exptl_absorpt_coefficient_mu    1.978
_exptl_absorpt_correction_T_max  'see above'
_exptl_absorpt_correction_T_min  'Tmin/tmax ratio 0.798486'
_exptl_absorpt_correction_type   'empirical, SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             326
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0282P)^2^+0.2590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                2556
_reflns_number_total             2979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301212n.txt
_cod_data_source_block           22jc
_cod_database_code               7050559