Syntheses, crystal structures and magnetic properties of di- and trinuclear croconato-bridged copper(ii) complexes
Castro, Isabel; Calatayud, María Luisa; Lloret, Francesc; Sletten, Jorunn; Julve, Miguel; Journal of the Chemical Society, Dalton Transactions  (2002) 2397–; doi:10.1039/b201090a

data_7011533
_publ_section_title
;
 Syntheses, crystal structures and magnetic properties of di- and
 trinuclear croconato-bridged copper(ii) complexes
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2397
_journal_paper_doi               10.1039/b201090a
_journal_year                    2002
_chemical_formula_sum            'C72 H40 Cu3 F6 N10 O16 S2'
_chemical_formula_weight         1669.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.604(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.2425(6)
_cell_length_b                   10.9029(5)
_cell_length_c                   21.8194(9)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     6556.8(4)
_computing_cell_refinement       'SAINT, version 4.0'
_computing_data_collection       'SMART, version 4.0'
_computing_data_reduction        'SAINT, version 4.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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  0.1339
_diffrn_reflns_av_sigmaI/netI    0.1609
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19107
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        1
_diffrn_standards_number
'50 first frames remeasured at end of experiment'
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  'see above'
_exptl_absorpt_correction_T_min  'ratio T_min/T_max 0.691378'
_exptl_absorpt_correction_type   'empirical, SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3372
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.2315
_refine_ls_R_factor_gt           0.0873
_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^)+(0.0667P)^2^+0.0000P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                2392
_reflns_number_total             5762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201090a.txt
_cod_data_source_block           cuphcrtf
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7011533