Oxacalix[3]arene Complexes with the ReI(CO)3Fragment†
Hinrichs, Matthias; Hofbauer, Florian R.; Klüfers, Peter; Suhanji, Mihael; Inorganic Chemistry 45 (2006) 6688–6693; doi:10.1021/ic0603048

data_4332378
_publ_section_title
;
 Oxacalix[3]arene Complexes with the ReI(CO)3Fragment&#x2020;
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6688
_journal_page_last               6693
_journal_paper_doi               10.1021/ic0603048
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source
;
Lab book number 3 A, entry 202
0.3 mmol 1,8-Diazabicyclo[5.4.0]undec-7-ene (DBU) (0.046 g) and 0.1 mmol
p-Methyl-Oxacalix[3]arene (p-Me-Oc[3]a) (0.045 g) are suspended in 4 mL
acetonitrile. Then 0.2 mmol (NET4)2[Re(CO)3Br3] (0.154 g) is added.
A white voluminous solid is formed right after addition of the DBU. The
suspension is stirred at room teperature for 5 hours. After 1 hour the solid
is completely solved. The acetonitrile is removed in vaccuo and the resulting
white to light yellow solid is dissolved in 2 mL of dry CH2Cl2. To crystallize
NEt4Br the solution is layered with Et2O and stored at 4 deg C. The next day
the  solution is filtered from the resulting white powder and the solution
is layered again with Et2O. After one day colourless crystals of [DBUH+1]Br
have appeared. These are filtered off and Et2O is added again. A white solid
appears which is filtered off and the resulting solution is layered with
hexane and stored at 4 deg C. After one month the solvent is completely
removed and colourless crystals have grown.
;
_chemical_formula_moiety
'4(C30 H28 O9 Re1), 4(C27 H30 O6), 4(C9 H17 N2)'
_chemical_formula_sum            'C264 H300 N8 O60 Re4'
_chemical_formula_weight         5290.053
_chemical_name_common            (DBUH+1)[Re(CO)3(p-Methyloxacalix[3]areneH-2)]
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_block_code                Re_CO_p-Me-Oc[3]a_DBUH+1_jn080_Hinrichs
_audit_creation_date             27-Feb-05
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                76.8060(5)
_cell_angle_beta                 83.1942(5)
_cell_angle_gamma                74.9826(7)
_cell_formula_units_Z            1
_cell_length_a                   16.6126(2)
_cell_length_b                   18.5955(3)
_cell_length_c                   23.9217(4)
_cell_measurement_reflns_used    74792
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     6935.23(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_collimation    0.35
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1575
_diffrn_reflns_av_sigmaI/netI    0.2776
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            93595
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.14
_diffrn_source_current           75.00
_diffrn_source_power             4.125
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_T_max  0.9536
_exptl_absorpt_correction_T_min  0.8002
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.26664(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1514
_refine_ls_number_reflns         31339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.2424
_refine_ls_R_factor_gt           0.0853
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2522
_reflns_number_gt                12343
_reflns_number_total             31339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0603048sup1.cif
_cod_data_source_block           1
_cod_database_code               4332378