NMR and X-ray crystallographic studies of unsymmetrical 25,26;27,28-dibridged para-tert-butyl calix[4]arene bisphosphites with a large “through-space” P–P coupling
Maji, Pathik; Krishnamurthy, Setharampattu S.; Nethaji, Munirathinam; New Journal of Chemistry 34 (2010) 1478–; doi:10.1039/b903771c

data_7053247
_publ_section_title
;
 NMR and X-ray crystallographic studies of unsymmetrical
 25,26;27,28-dibridged para-tert-butyl calix[4]arene bisphosphites with a
 large &#x201C;through-space&#x201D; P--P coupling
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1478
_journal_paper_doi               10.1039/b903771c
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C56 H71 O5 P'
_chemical_formula_sum            'C56 H71 O5 P'
_chemical_formula_weight         855.10
_chemical_name_common
;
5,11,17,23-tetra-(tert-butyl)calix(4)arene 25,26-
(dihydroxy)(27,28-(2,6-di-isopropyl-phenyl)) monophosphite
;
_chemical_name_systematic
;
5,11,17,23-tetra-(tert-butyl)calix[4]arene
25,26-(dihydroxy){27,28-(2,6-di-isopropyl-phenyl)}
monophosphite
;
_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                90.000(5)
_cell_angle_beta                 91.060(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   10.280(5)
_cell_length_b                   27.784(5)
_cell_length_c                   17.984(5)
_cell_measurement_reflns_used    356
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.50
_cell_volume                     5136(3)
_computing_cell_refinement       'BRUKER SMART APEX CCD'
_computing_data_collection       'BRUKER SMART APEX CCD'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'WINGX V1.80.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD'
_diffrn_measurement_method       OMEGA
_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  0.1786
_diffrn_reflns_av_sigmaI/netI    0.1840
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36813
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9730
_exptl_absorpt_correction_T_min  0.9636
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       RECTANGULAR
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     583
_refine_ls_number_reflns         9034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.2505
_refine_ls_R_factor_gt           0.1108
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1909P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2604
_refine_ls_wR_factor_ref         0.3289
_reflns_number_gt                3663
_reflns_number_total             9034
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b903771c.txt
_cod_data_source_block           pat22n_m
_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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7053247