Synthesis, structure and magnetism of a unique dodecanuclearcopper(ii) 'picture frame' held in a 4 × 4 grid-like assembly
Matthews, Craig J.; Onions, Stuart T.; Morata, Gérald; Salvia, Margarita Bosch; Elsegood, Mark R. J.; Price, Daniel J.; Chemical Communications (Cambridge, United Kingdom)  (2003) 320–321; doi:10.1039/b210891g

data_7103957
_publ_section_title
;
 Synthesis, structure and magnetism of a unique dodecanuclearcopper(ii)
 'picture frame' held in a 4 \\times 4 grid-like assembly
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   3
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              320
_journal_page_last               321
_journal_paper_doi               10.1039/b210891g
_journal_year                    2003
_chemical_formula_sum            'C146 H172 B9 Cu12 F36 N80 Na O39'
_chemical_formula_weight         5238.40
_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-97
_cell_angle_alpha                75.286(2)
_cell_angle_beta                 77.638(2)
_cell_angle_gamma                65.984(2)
_cell_formula_units_Z            2
_cell_length_a                   21.3049(11)
_cell_length_b                   21.3272(11)
_cell_length_c                   24.7637(13)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.18
_cell_volume                     9862.5(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.1138
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74145
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, G.M.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.199
_refine_diff_density_min         -1.188
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.00044(9)
_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   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2864
_refine_ls_number_reflns         25752
_refine_ls_number_restraints     1317
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1544P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2251
_refine_ls_wR_factor_ref         0.2543
_reflns_number_gt                13846
_reflns_number_total             25752
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b210891g.txt
_cod_data_source_block           cjm4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7103957