Calix[4]arene Ligands with Phosphorus-Containing Groups Tethered at the Upper Rim
Izilda A. Bagatin; Dominique Matt; Holger Thönnessen; Peter G. Jones; Inorganic Chemistry 38 (1999) 1585–1591; doi:10.1021/ic980964f

data_4321865
_publ_section_title
;
 Calix[4]arene Ligands with Phosphorus-Containing Groups Tethered at the
 Upper Rim
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1585
_journal_page_last               1591
_journal_paper_doi               10.1021/ic980964f
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C80.5 H96.5 Cl7.5 O10 P2'
_chemical_formula_weight         1551.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.04(2)
_cell_angle_beta                 93.13(2)
_cell_angle_gamma                100.268(18)
_cell_formula_units_Z            2
_cell_length_a                   16.313(5)
_cell_length_b                   16.553(5)
_cell_length_c                   17.068(6)
_cell_measurement_temperature    173(2)
_cell_volume                     4282(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15336
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  0.9057
_exptl_absorpt_correction_T_min  0.8107
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1634
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.0000(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         14801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.162
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2464
_reflns_number_gt                7841
_reflns_number_total             14801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980964f.cif
_cod_data_source_block           izil
_cod_original_cell_volume        4283(2)
_cod_original_formula_sum        'C80.50 H96.50 Cl7.50 O10 P2'
_cod_database_code               4321865