Hexanuclear Copper(II) Cages Built on a Central {μ3-O...H...μ3-O} Moiety, 1,3-Bis(dimethylamino)-2-propanolato and Capping R-phosphonates: Crystal Structures, Magnetic Behavior, and DFT Studies
Saskia Speed; Ramon Vicente; Daniel Aravena; Eliseo Ruiz; Olivier Roubeau; Simon J. Teat; M. Salah El Fallah; Inorganic Chemistry 51 (2012) 6842–6850; doi:10.1021/ic300589h

data_4329505
_publ_section_title
;
 Hexanuclear Copper(II) Cages Built on a Central {\m3-O...H...\m3-O}
 Moiety, 1,3-Bis(dimethylamino)-2-propanolato and Capping R-phosphonates:
 Crystal Structures, Magnetic Behavior, and DFT Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6842
_journal_page_last               6850
_journal_paper_doi               10.1021/ic300589h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C66 H124 Cl4 Cu12 N12 O40 P4, 10(H2 O)'
_chemical_formula_sum            'C66 H144 Cl4 Cu12 N12 O50 P4'
_chemical_formula_weight         2924.24
_chemical_name_systematic
;  
 ?  
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.422(3)
_cell_length_b                   20.250(4)
_cell_length_c                   35.116(7)
_cell_measurement_reflns_used    238
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.8
_cell_volume                     10967(4)
_computing_cell_refinement       'HKL2000 (Z. Otwinowski and W. Minor, 1997)'
_computing_data_collection       MxCube
_computing_data_reduction        'HKL2000 (Z. Otwinowski and W. Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type
'single-axis HUBER diffractometer with ADSC Q210r CCD detector'
_diffrn_measurement_method       '  phi rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'ESRF BM16'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75140
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            43916
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    2.949
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   MULABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       block
_exptl_crystal_F_000             5937
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.879
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       0.00343(17)
_refine_ls_extinction_expression 'Fc*=kFc[1+0.001xFc2 l3/sin(2  q)]-1/4'
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         13079
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0597
_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/[  s2(Fo2)+(0.0930P)2+44.3374P] where P=(Fo2+2Fc2)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1633
_reflns_number_gt                12125
_reflns_number_total             13079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300589h_si_001_1.cif
_cod_data_source_block           ss209
_cod_database_code               4329505