Calix[4]arene-fused phospholes
Elaieb, Fethi; Sémeril, David; Matt, Dominique; Pfeffer, Michel; Bouit, Pierre-Antoine; Hissler, Muriel; Gourlaouen, Christophe; Harrowfield, Jack; Dalton Trans.  (2017) –; doi:10.1039/C7DT01899A

data_7043533
_publ_section_title
;
 Calix[4]arene-fused phospholes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01899A
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C52 H55 O5 P'
_chemical_formula_sum            'C52 H55 O5 P'
_chemical_formula_weight         790.93
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           199
_space_group_name_Hall           'I 2b 2c 3'
_space_group_name_H-M_alt        'I 21 3'
_symmetry_space_group_name_Hall  'I 2b 2c 3'
_symmetry_space_group_name_H-M   'I 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-04-21 deposited with the CCDC.
2017-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            48
_cell_length_a                   38.0572(4)
_cell_length_b                   38.0572(4)
_cell_length_c                   38.0572(4)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      63.56
_cell_measurement_theta_min      4.02
_cell_volume                     55120.2(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            161417
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.704
_diffrn_reflns_theta_min         2.322
_diffrn_source                   'Cu-ImuS microfocus tube'
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             20256
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
The residual electron density was assigned to half a molecule of hexane [599/24= 25 e per asymmetric unit; half a molecule of C6H14 would give 25 e]. 
;
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         16277
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+11.7206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13929
_reflns_number_total             16277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01899a2.cif
_cod_data_source_block           dmfe160201
_cod_original_cell_volume        55120.2(17)
_cod_database_code               7043533
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.902
_shelxl_version_number           2013-4
_shelx_res_checksum              81726