Self-assembled polymetallic square grids ([2 ? 2] M4, [3 ? 3] M9) and trigonal bipyramidal clusters (M5)?structural and magnetic properties
Dawe, Louise N.; Abedin, Tareque S. M.; Kelly, Timothy L.; Thompson, Laurence K.; Miller, David O.; Zhao, Liang; Wilson, Claire; Leech, Michael A.; Howard, Judith A. K.; Journal of Materials Chemistry 16 (2006) 2645–; doi:10.1039/b602595a

data_7203328
_publ_section_title
;
 Self-assembled polymetallic square grids ([2 ? 2] M4, [3 ? 3] M9) and
 trigonal bipyramidal clusters (M5)?structural and magnetic properties
;
_journal_issue                   26
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2645
_journal_paper_doi               10.1039/b602595a
_journal_volume                  16
_journal_year                    2006
_chemical_formula_sum            'C46 H49 Cl4 Cu4 N31 O20'
_chemical_formula_weight         1752.08
_chemical_name_systematic
;
?
;
_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                 128.679(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.912(9)
_cell_length_b                   21.105(7)
_cell_length_c                   18.184(7)
_cell_measurement_reflns_used    14019
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.8190
_cell_measurement_theta_min      1.9298
_cell_volume                     6864(4)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_publication_material  'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_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  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37116
_diffrn_reflns_theta_full        31.01
_diffrn_reflns_theta_max         31.01
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_T_max  0.8358
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.00010(12)
_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   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.1101
_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^)+(0.1466P)^2^+53.5329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2878
_refine_ls_wR_factor_ref         0.2986
_reflns_number_gt                8054
_reflns_number_total             9417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602595a.txt
_cod_data_source_block           shelxl(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7203328