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_7043530
_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 ad
_chemical_formula_moiety         'C52 H55 Au Cl O4 P'
_chemical_formula_sum            'C52 H55 Au Cl O4 P'
_chemical_formula_weight         1007.34
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 99.456(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0854(9)
_cell_length_b                   18.1789(19)
_cell_length_c                   13.8937(15)
_cell_measurement_reflns_used    6190
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.27
_cell_volume                     2263.5(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.1090
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22333
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.029
_diffrn_reflns_theta_min         1.861
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.389
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.370
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 3099 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.033(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         10857
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                8350
_reflns_number_total             10857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01899a2.cif
_cod_data_source_block           dmfe151216
_cod_database_code               7043530
_shelx_estimated_absorpt_t_min   0.581
_shelx_estimated_absorpt_t_max   0.849
_shelxl_version_number           2013-4
_shelx_res_checksum              54985