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_4112187
_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            'C72 H74 Br2 Mo2 N4 O12'
_chemical_formula_weight         1539.05
_chemical_name_common            Mo2(DAniF)2(Calix[4]aren
_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                106.9900(10)
_cell_angle_beta                 95.5590(10)
_cell_angle_gamma                105.8630(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1936(8)
_cell_length_b                   14.4964(10)
_cell_length_c                   20.9932(14)
_cell_measurement_reflns_used    7561
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.434
_cell_measurement_theta_min      2.214
_cell_volume                     3350.1(4)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21633
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.8538
_exptl_absorpt_correction_T_min  0.4409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       needle
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         14928
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+3.4727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                10591
_reflns_number_total             14928
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja0396899si20031206_035237_5.cif
_cod_data_source_block           3
_cod_database_code               4112187