Synthesis, crystal structure and magnetic properties of the triangulo-tricopper(ii) complex [Cu3(cpse)3(H2O)3]·8.5H2O
López-Sandoval, Horacio; Contreras, Rosalinda; Escuer, Albert; Vicente, Ramon; Bernès, Sylvain; Nöth, Heinrich; Jeffery Leigh, G.; Barba-Behrens, Noráh; Journal of the Chemical Society, Dalton Transactions  (2002) 2648–; doi:10.1039/b110915b

data_7702774
_publ_section_title
;
 Synthesis, crystal structure and magnetic properties of the
 triangulo-tricopper(ii) complex [Cu3(cpse)3(H2O)3]&#x00B7;8.5H2O
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2648
_journal_paper_doi               10.1039/b110915b
_journal_year                    2002
_chemical_formula_sum            'C36 H68 Cu3 N3 O20.5'
_chemical_formula_weight         1061.55
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '2001-05-08 l'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.1559(1)
_cell_length_b                   15.1559(1)
_cell_length_c                   37.3630(7)
_cell_measurement_temperature    183(2)
_cell_volume                     7432.52(16)
_computing_molecular_graphics    'SHELXTL 5.10 (Sheldrick, 1998)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL 5.10 (Sheldrick, 1998)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector                 'Area CCD'
_diffrn_measured_fraction_theta_full 0.720
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14234
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.90769
_exptl_absorpt_correction_T_min  0.80545
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             3336
_exptl_crystal_preparation
;
Crystal mounted on glass fiber with perfluorpolyetheroil
;
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(13)
_refine_ls_extinction_coef       0.00015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0347P)^2^+8.2073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                2745
_reflns_number_total             3010
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b110915b.txt
_cod_data_source_block           noeth48
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_hydrogens' value 'geom + difmap' was
changed to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        7432.51(14)
_cod_original_sg_symbol_H-M      R32
_cod_original_formula_sum        'C36 H68 Cu3 N3 O20.50'
_cod_database_code               7702774