Nonemployed Simple Carboxylate Ions in Well-Investigated Areas of Heterometallic Carboxylate Cluster Chemistry: A New Family of {Cu(II)4Ln(III)8} Complexes Bearing tert-Butylacetate Bridging Ligands.
Dermitzaki, Despina; Raptopoulou, Catherine P.; Psycharis, Vassilis; Escuer, Albert; Perlepes, Spyros P.; Stamatatos, Theocharis C.; Inorganic chemistry 54 (2015) 7555–7561; doi:10.1021/acs.inorgchem.5b01179

data_4346281
_publ_section_title
;
 Nonemployed Simple Carboxylate Ions in Well-Investigated Areas of
 Heterometallic Carboxylate Cluster Chemistry: A New Family of
 {Cu(II)4Ln(III)8} Complexes Bearing tert-Butylacetate Bridging Ligands.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7555
_journal_page_last               7561
_journal_paper_doi               10.1021/acs.inorgchem.5b01179
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C131.2 H223.2 Cu4 Gd8 N9.4 O53.1'
_chemical_formula_weight         4294.15
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                93.3240(10)
_cell_angle_beta                 113.4450(10)
_cell_angle_gamma                99.8430(10)
_cell_formula_units_Z            1
_cell_length_a                   16.1708(3)
_cell_length_b                   17.2594(3)
_cell_length_c                   18.8906(3)
_cell_measurement_reflns_used    51577
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      71.99
_cell_measurement_theta_min      6.53
_cell_volume                     4719.34(15)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            71127
_diffrn_reflns_theta_full        62.50
_diffrn_reflns_theta_max         62.50
_diffrn_reflns_theta_min         6.53
_exptl_absorpt_coefficient_mu    18.892
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2129
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.733
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         14336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0946P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1799
_reflns_number_gt                10524
_reflns_number_total             14336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01179_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4719.33(14)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C131.20 H223.20 Cu4 Gd8 N9.40 O53.10'
_cod_database_code               4346281