Two Polymeric Compounds Built from Mononuclear and Tetrameric Squarate-Copper(II) Complexes by Deprotonation of 3,3-Bis(2-imidazolyl)propionic Acid (HBIP). Synthesis, Crystal Structure, and Magnetic Characterization of [Cu(HBIP)(BIP)](C4O4)1/2.2H2O and [{Cu(BIP)(OH2)}4(μ-C4O4)](ClO4)2.4H2O
Youness Akhriff; Juan Server-Carrió; Amparo Sancho; Julia García-Lozano; Emilio Escrivá; Lucía Soto; Inorganic Chemistry 40 (2001) 6832–6840; doi:10.1021/ic0106571

data_4320723
_publ_section_title
;
 Two Polymeric Compounds Built from Mononuclear and Tetrameric
 Squarate-Copper(II) Complexes by Deprotonation of
 3,3-Bis(2-imidazolyl)propionic Acid (HBIP). Synthesis, Crystal Structure,
 and Magnetic Characterization of [Cu(HBIP)(BIP)](C4O4)1/2.2H2O and
 [{Cu(BIP)(OH2)}4(\m-C4O4)](ClO4)2.4H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6832
_journal_page_last               6840
_journal_paper_doi               10.1021/ic0106571
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C40 H52 Cl2 Cu4 N16 O28'
_chemical_formula_weight         1530.04
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.13(1)
_cell_angle_beta                 80.14(1)
_cell_angle_gamma                84.02(1)
_cell_formula_units_Z            1
_cell_length_a                   8.010(1)
_cell_length_b                   13.073(1)
_cell_length_c                   14.561(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      10
_cell_volume                     1427.6(2)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 EXPRESS'
_computing_data_reduction        'XRAY76 (stewart, 1976)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'Omega-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0085
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5591
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.667
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Walker et al., 1983)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.564
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0781P)^2^+1.9693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                4177
_reflns_number_total             5029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0106571_2.cif
_cod_data_source_block           '[{Cu(BIP)(OH2)}4(m-C4O4)](ClO4).4H2O'
_cod_database_code               4320723