Installing Tungsten Fischer Carbene Complexes into a Calixarene Framework
D'Acunto, Maria Antonietta; Tommasone, Stefano; Talotta, Carmen; Brancatelli, Giovanna; Geremia, Silvano; Valletta, Elena; Marino-Merlo, Francesca; Macchi, Beatrice; Gaeta, Carmine; Neri, Placido; Spinella, Aldo; RSC Adv.  (2016) –; doi:10.1039/C6RA17326H

data_7226118
_publ_section_title
;
 Installing Tungsten Fischer Carbene Complexes into a Calixarene Framework
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA17326H
_journal_year                    2016
_chemical_formula_sum            'C73.6 H99.2 N2 O10 W'
_chemical_formula_weight         1355.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1k80b5
_audit_creation_date             2015-11-18T11:48:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-11-18 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.70(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.582(2)
_cell_length_b                   26.982(5)
_cell_length_c                   25.802(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.665
_cell_measurement_theta_min      10.081
_cell_measurement_wavelength     0.7
_cell_volume                     7342(2)
_computing_molecular_graphics    Pymol
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SIR2011, updated version of SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_wavelength     0.7
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_number            17886
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.665
_diffrn_reflns_theta_min         10.081
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_T_max  1.1208
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             2835
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.32
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0056(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         17886
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+4.3887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.081
_reflns_Friedel_coverage         0
_reflns_number_gt                16257
_reflns_number_total             17886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra17326h2.cif
_cod_data_source_block           Calix_W2
_cod_original_cell_volume        7342(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C73.60 H99.20 N2 O10 W'
_cod_database_code               7226118
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.848
_shelx_res_checksum              45583