Ferro- and Antiferromagnetic Coupling through 1,n-Dithiosquarate Bridges (n= 2, 3) in Copper(II) Dimers. Syntheses, Crystal Structures, and Magnetic Properties of [Cu2(bpca)2(1,2-dtsq)(H2O)].2H2O and [Cu2(bpca)2(1,3-dtsq)].2H2O
Isabel Castro; María Luisa Calatayud; Jorunn Sletten; Francesc Lloret; Juan Cano; Miguel Julve; Gunther Seitz; Klaus Mann; Inorganic Chemistry 38 (1999) 4680–4687; doi:10.1021/ic9904384

data_4322312
_publ_section_title
;
 Ferro- and Antiferromagnetic Coupling through 1,n-Dithiosquarate Bridges
 (n= 2, 3) in Copper(II) Dimers. Syntheses, Crystal Structures, and
 Magnetic Properties of [Cu2(bpca)2(1,2-dtsq)(H2O)].2H2O and
 [Cu2(bpca)2(1,3-dtsq)].2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4680
_journal_page_last               4687
_journal_paper_doi               10.1021/ic9904384
_journal_volume                  38
_journal_year                    1999
_chemical_formula_analytical     'C28 H22 Cu2 N6 O9 S2'
_chemical_formula_moiety         'C28 H22 Cu2 N6 O9 S2'
_chemical_formula_structural     'C28 H22 Cu2 N6 O9 S2'
_chemical_formula_sum            'C28 H22 Cu2 N6 O9 S2'
_chemical_formula_weight         777.72
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.276(2)
_cell_angle_beta                 100.009(2)
_cell_angle_gamma                94.139(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3243(4)
_cell_length_b                   10.9036(5)
_cell_length_c                   15.5432(4)
_cell_measurement_temperature    223(2)
_cell_volume                     1551.90(11)
_computing_cell_refinement       'SAINT, version 4.0'
_computing_data_collection       'SMART, version 4.0'
_computing_data_reduction        'SAINT, version 4.0'
_computing_molecular_graphics    XP-97
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       '2K Smart CCD'
_diffrn_measurement_method       \w
_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  0.1067
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24800
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time
;
        50 first frames remeasured at end ofdata collection
;
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   'numerical integration'
_exptl_crystal_colour            'brownish green'
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       no
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.014
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_obs          0.0662
_refine_ls_shift/esd_max         0.123
_refine_ls_shift/esd_mean        0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+2.9629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1854
_refine_ls_wR_factor_obs         0.1612
_reflns_number_observed          5033
_reflns_number_total             7737
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9904384_1.cif
_cod_data_source_block           cu12dtsq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+2.9629P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+2.9629P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322312