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_7226119
_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 H98 N2 O10 W'
_chemical_formula_weight         1347.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1k8fcm
_audit_creation_date             2015-11-20T11:54:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-11-20 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.056(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.439(1)
_cell_length_b                   18.945(1)
_cell_length_c                   26.776(2)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.835
_cell_measurement_theta_min      5.071
_cell_measurement_wavelength     0.7
_cell_volume                     7105.2(8)
_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 0.863
_diffrn_measured_fraction_theta_max 0.864
_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_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.05
_diffrn_reflns_Laue_measured_fraction_full 0.863
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17984
_diffrn_reflns_point_group_measured_fraction_full 0.863
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         5.071
_exptl_absorpt_coefficient_mu    1.606
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.28
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0309(12)
_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   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         11316
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+35.3279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0
_reflns_number_gt                10497
_reflns_number_total             11316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra17326h2.cif
_cod_data_source_block           Calix_W1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7226119
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.882
_shelx_res_checksum              27670