Self-Assembled Supramolecular Clusters Based on Phosphines and Coinage Metals: Tetrahedra, Helicates, and Mesocates
Sang Ho Lim; Seth M. Cohen; Inorganic Chemistry 52 (2013) 7862–7872; doi:10.1021/ic302840x

data_4335426
_publ_section_title
;
 Self-Assembled Supramolecular Clusters Based on Phosphines and Coinage
 Metals: Tetrahedra, Helicates, and Mesocates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7862
_journal_page_last               7872
_journal_paper_doi               10.1021/ic302840x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C264 H180 Cu4 I4 P12, 3(C H2 Cl2)'
_chemical_formula_sum            'C267 H186 Cl6 Cu4 I4 P12'
_chemical_formula_weight         4740.31
_chemical_name_common            CH2Cl2@[Cu4(tppepb)4]I4
_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                 114.534(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.8818(15)
_cell_length_b                   49.512(2)
_cell_length_c                   19.2091(9)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.45
_cell_measurement_theta_min      3.01
_cell_volume                     30180(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15310
_diffrn_reflns_theta_full        50.72
_diffrn_reflns_theta_max         50.72
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    4.941
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_description       block
_exptl_crystal_F_000             9592
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         15310
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1236P)^2^+30.8811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.2002
_reflns_number_gt                11800
_reflns_number_total             15310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302840x_si_002_01.cif
_cod_data_source_block           CH2Cl2@[Cu4[tppepb]4]I4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4335426