A Calix[4]arene Carceplex with Four Rh24+ Fasteners
F. Albert Cotton; Peng Lei; Chun Lin; Carlos A. Murillo; Xiaoping Wang; Shu-Yan Yu; Zhong-Xing Zhang; Journal of the American Chemical Society 126 (2004) 1518–1525; doi:10.1021/ja0396899

data_4112186
_publ_section_title
;
 A Calix[4]arene Carceplex with Four Rh24+ Fasteners
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1518
_journal_page_last               1525
_journal_paper_doi               10.1021/ja0396899
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C73 H78 Br2 N4 O13 Rh2'
_chemical_formula_weight         1585.03
_chemical_name_common            Rh2(DAniF)2(calixarene-dicarboxy)
_chemical_name_systematic
; 
 ? 
;
_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                77.8510(10)
_cell_angle_beta                 77.7490(10)
_cell_angle_gamma                80.1740(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0208(6)
_cell_length_b                   13.1643(6)
_cell_length_c                   23.1380(11)
_cell_measurement_reflns_used    9539
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.484
_cell_measurement_theta_min      2.448
_cell_volume                     3467.4(3)
_computing_cell_refinement       'SAINT V. 6.22'
_computing_data_collection       'SMART V.5618'
_computing_data_reduction        'SAINT V. 6.22'
_computing_molecular_graphics    'SHELXTL (siemens, 1996)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Brucker SMART 1000 CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23063
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.694
_exptl_absorpt_correction_T_max  0.7616
_exptl_absorpt_correction_T_min  0.6305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.03'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         15357
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+0.4378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                11518
_reflns_number_total             15357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0396899si20031206_035237_4.cif
_cod_data_source_block           2MeOH
_cod_database_code               4112186