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_4310928
_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            'C62 H74 Cl2 O5 P2'
_chemical_formula_weight         1032.05
_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                102.288(7)
_cell_angle_beta                 102.074(8)
_cell_angle_gamma                96.007(8)
_cell_formula_units_Z            2
_cell_length_a                   14.353(1)
_cell_length_b                   14.612(1)
_cell_length_c                   14.916(1)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      15.00
_cell_measurement_theta_min      10.29
_cell_volume                     2952.3(4)
_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      230(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.026
_diffrn_reflns_av_sigmaI/netI    0.091
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10718
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        8.49
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.210
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.403
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         10269
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.151
_refine_ls_R_factor_gt           0.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1452P)^2^+0.9571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.228
_refine_ls_wR_factor_ref         0.260
_reflns_number_gt                5965
_reflns_number_total             10269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035359dsi20031124_025643_3.cif
_cod_data_source_block           3(mhclxpcl)
_cod_original_cell_volume        2952.3(3)
_cod_original_formula_sum        '[C55 H66 Cl2 O5 P2] . [C7 H8]'
_cod_database_code               4310928