Synthesis, Structures, And Magnetic Behavior of New Anionic Copper(II) Sulfate Aggregates and Chains
Andrew D. Burrows; Mary F. Mahon; Viorica M. Sebestyen; Yanhua Lan; Annie K. Powell; Inorganic Chemistry 51 (2012) 10983–10989; doi:10.1021/ic301478x

data_4330670
_publ_contact_author_address
;Department of Chemistry,
University of Bath,
Claverton Down,
Bath,
UK
BA2 7AY
;
_publ_contact_author_name        'Andrew D. Burrows'
_publ_section_title
;
 Synthesis, Structures, And Magnetic Behavior of New Anionic Copper(II)
 Sulfate Aggregates and Chains
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10983
_journal_page_last               10989
_journal_paper_doi               10.1021/ic301478x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C20 H60 Cu6 N8 O30 S6'
_chemical_formula_weight         1466.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.183(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.1050(3)
_cell_length_b                   10.5140(2)
_cell_length_c                   18.7530(5)
_cell_measurement_reflns_used    114666
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2515.81(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV 1997-2004)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski, Minor 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1191
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39253
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    2.836
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.936
_exptl_crystal_description       needle
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.344
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0503P)^2^+8.2479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                4248
_reflns_number_total             5766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301478x_si_002_1.cif
_cod_data_source_block           k09adb19
_cod_database_code               4330670