Phosphorus-Based p-tert-Butylcalix[5]arene Ligands
Paul Sood; Mohan Koutha; Maomian Fan; Yaroslav Klichko; Hongming Zhang; Michael Lattman; Inorganic Chemistry 43 (2004) 2975–2980; doi:10.1021/ic035359d

data_4310927
_publ_section_title
;
 Phosphorus-Based p-tert-Butylcalix[5]arene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2975
_journal_page_last               2980
_journal_paper_doi               10.1021/ic035359d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C81 H92 O5 P2'
_chemical_formula_weight         1207.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.621(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.269(1)
_cell_length_b                   24.363(1)
_cell_length_c                   17.584(1)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     6968.5(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      228(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\g/\w scans'
_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  0.036
_diffrn_reflns_av_sigmaI/netI    0.052
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7769
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        6.89
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   n/a
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0055(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   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         7461
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.105
_refine_ls_R_factor_gt           0.076
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+11.8480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.206
_refine_ls_wR_factor_ref         0.223
_reflns_number_gt                5455
_reflns_number_total             7461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035359dsi20031124_025643_2.cif
_cod_data_source_block           2(ps-p14-2)
_cod_original_cell_volume        6968.4(6)
_cod_original_formula_sum        '[C67 H76 O5 P2] . 2[C7 H8]'
_cod_database_code               4310927