Synthesis of a resorcinarene-based tetraphosphine-cavitand and its use in Heck reactions
Moll, Hani El; Sémeril, David; Matt, Dominique; Youinou, Marie-Thérèse; Toupet, Loïc; Organic & Biomolecular Chemistry 7 (2009) 495–501; doi:10.1039/b813373e

data_7150526
_publ_section_title
;
 Synthesis of a resorcinarene-based tetraphosphine-cavitand and its use
 in Heck reactions
;
_journal_issue                   3
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              495
_journal_page_last               501
_journal_paper_doi               10.1039/b813373e
_journal_volume                  7
_journal_year                    2009
_chemical_formula_moiety         '(C104 H108 O8 P4) . 4(C H4 O)'
_chemical_formula_sum            'C108 H124 O12 P4'
_chemical_formula_weight         1737.95
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.999(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.2736(10)
_cell_length_b                   16.3323(9)
_cell_length_c                   24.0996(10)
_cell_measurement_temperature    90(2)
_cell_volume                     9565.0(9)
_computing_cell_refinement
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26'
_computing_data_collection
'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26'
_computing_data_reduction
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26'
_computing_molecular_graphics    'PLATON_(Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1998)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 19.64
_diffrn_measured_fraction_theta_full 0.870
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'CCD Saphire 3 Xcalibur'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.2095
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33109
_diffrn_reflns_theta_full        31.99
_diffrn_reflns_theta_max         31.99
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.752
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         17322
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.755
_refine_ls_R_factor_all          0.1643
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                6024
_reflns_number_total             17322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813373e.txt
_cod_data_source_block           he43dry
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        9565.0(7)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7150526