A p-tert-butylcalix[6]arene bearing phosphinoyl pendant arms for the complexation and sensitisation of lanthanide ions
Flor de María Ramírez; Sabi Varbanov; Corine Cécile; Gilles Muller; Nicolas Fatin-Rouge; Rosario Scopelliti; Jean-Claude G. Bünzli; J. Chem. Soc., Dalton Trans.  (2002) 4505–4513; doi:10.1039/b206238k

data_7011976
_publ_section_title
;
 A p-tert-butylcalix[6]arene bearing phosphinoyl pendant arms for the
 complexation and sensitisation of lanthanide ions
;
_journal_issue                   23
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4505
_journal_page_last               4513
_journal_paper_doi               10.1039/b206238k
_journal_year                    2002
_chemical_formula_moiety         'C84 H126 O12 P6, 0.5(C7 H8), 13(H2 O)'
_chemical_formula_sum            'C87.5 H156 O25 P6'
_chemical_formula_weight         1793.94
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.552(11)
_cell_length_b                   30.500(14)
_cell_length_c                   27.111(3)
_cell_measurement_reflns_used    909
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      10.98455
_cell_measurement_theta_min      1.35455
_cell_volume                     20420(13)
_computing_cell_refinement
'Oxford Diffraction CrysAlis RED, release 1.6.9 beta'
_computing_data_collection       'marresearch mar345, release 1.2.11'
_computing_data_reduction
'Oxford Diffraction CrysAlis RED, release 1.6.9 beta'
_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      143(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'marresearch mar345 IPDS'
_diffrn_measurement_method
'60 images with deltaphi = 3 degrees and exp. time = 180 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1938
_diffrn_reflns_av_sigmaI/netI    0.3410
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            104975
_diffrn_reflns_theta_full        24.54
_diffrn_reflns_theta_max         24.54
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             7768
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.786
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1985
_refine_ls_number_reflns         31919
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.787
_refine_ls_R_factor_all          0.3105
_refine_ls_R_factor_gt           0.1035
_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^)+(0.1340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2414
_refine_ls_wR_factor_ref         0.3378
_reflns_number_gt                6138
_reflns_number_total             31919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206238k.txt
_cod_data_source_block           bunz47
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        20419(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C87.50 H156 O25 P6'
_cod_database_code               7011976