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_4332379
_publ_section_title
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 Oxacalix[3]arene Complexes with the ReI(CO)3Fragment&#x2020;
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_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
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Lab book number 3 A, entry 205
The synthesis is carried out under nitrogen atmposphere with dried and
desoxygenated acetonitrile.
0.1 mmol (NET4)2[Re(CO)3Br3] (0.077 g) and 0.1 mmol p-Isopropyl-Oxacalix[3]arene
(p-IPr-Oc[3]a) (0.053 g) are suspended in 2 mL acetonitrile. Then 0.3 mmol 1,8-
Diazabicyclo[5.4.0]undec-7-ene (DBU) (0.046 g) is added. A white voluminous
solid is formed right after addition of the DBU). The suspension is heated to 85
deg C. The solid dissolves at about 70 deg C. It is heated for 5 hours in
which again a white solid appears. After cooling the mixture to room
temperature nitrogen atmosphere is no longer needed. After filtration the
light yellow solution is treated with a few drops of water in which a white
solid appears, that could be redissolved by shaking. After filtration the
solution hold on 4 deg C. Colourless needles are formed after 1 hour.
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_chemical_formula_moiety
'4(C33 H42 O6), 4(C36 H40 O9 Re1), 4(C8 H20 N), 2(C2 H3 N1)'
_chemical_formula_sum            'C312 H414 N6 O60 Re4'
_chemical_formula_weight         5953.458
_chemical_name_common            (NEt4)[Re(CO)3(p-Isopropyloxacalix[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-IPr-Oc[3]a_NET4_jn044_Hinrichs
_audit_creation_date             01-Feb-05
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                109.9521(6)
_cell_angle_beta                 100.2614(6)
_cell_angle_gamma                96.7309(6)
_cell_formula_units_Z            1
_cell_length_a                   14.1272(2)
_cell_length_b                   23.5791(4)
_cell_length_c                   24.6058(5)
_cell_measurement_reflns_used    99764
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     7439.5(2)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1819
_diffrn_reflns_av_sigmaI/netI    0.2949
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            103208
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.15
_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    1.698
_exptl_absorpt_correction_T_max  0.8844
_exptl_absorpt_correction_T_min  0.7403
_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    1.32887(4)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1722
_refine_ls_number_reflns         33287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.2801
_refine_ls_R_factor_gt           0.0952
_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          0.1759
_refine_ls_wR_factor_ref         0.2352
_reflns_number_gt                11835
_reflns_number_total             33287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0603048sup1.cif
_cod_data_source_block           2
_cod_database_code               4332379