Combining Dynamic Heteroleptic Complex Formation with Constitutional Dynamic Synthesis: A Facile Way to M3LL' Cage Assemblies
Jian Fan; Jan W. Bats; Michael Schmittel; Inorganic Chemistry 48 (2009) 6338–6340; doi:10.1021/ic9008366

data_4302773
_publ_contact_author_address
;
 Center for Micro- and Nanochemistry and Engineering
 Organische Chemie I
 Universit\"at Siegen
 Adolf-Reichwein-Strasse
 D-57068 Siegen
 Germany
;
_publ_contact_author_email       schmittel@chemie.uni-siegen.de
_publ_contact_author_fax         '+49 271 7403270'
_publ_contact_author_name        'Michael Schmittel'
_publ_contact_author_phone       '+49 271 7404356'
_publ_section_title
;
Combining Dynamic Heteroleptic Complex Formation with Constitutional
Dynamic Synthesis: A Facile Way to M3LL' Cage Assemblies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6338
_journal_page_last               6340
_journal_paper_doi               10.1021/ic9008366
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C78 H70 Cu2 N8 , 2 ( P F6) , 2 (C H2 Cl2)'
_chemical_formula_sum            'C80 H74 Cl4 Cu2 F12 N8 P2'
_chemical_formula_weight         1706.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.990(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3929(9)
_cell_length_b                   27.050(3)
_cell_length_c                   13.6162(13)
_cell_measurement_reflns_used    303
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     3790.7(6)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  SIEMENS_SMART_CCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            55611
_diffrn_reflns_theta_full        27.2
_diffrn_reflns_theta_max         28.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  1200
_diffrn_standards_number         537
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ' SHELXTL (sheldrick, 1996)'
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+2.5P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                6117
_reflns_number_total             8738
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic9008366_si_001_1.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        3790.8(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4302773