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_7053246
_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         'C59 H79 O6 P'
_chemical_formula_sum            'C59 H79 O6 P'
_chemical_formula_weight         915.19
_chemical_name_common
;
5,11,17,23-tetra-(tert-butyl)calix(4)arene 25,26-
(dihydroxy)(27,28-(2,6-di-tert-butyl-4-methyl-
phenyl))monophosphite,monohydrate
;
_chemical_name_systematic
;
5,11,17,23-tetra-(tert-butyl)calix[4]arene
25,26-(dihydroxy){27,28-(2,6-di-tert-butyl-
4-methyl-phenyl)}monophosphite,monohydrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 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                 108.889(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.929(3)
_cell_length_b                   21.378(3)
_cell_length_c                   18.173(2)
_cell_measurement_reflns_used    378
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.50
_cell_volume                     5487.6(15)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19854
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.9714
_exptl_absorpt_correction_T_min  0.9549
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       RECTANGULAR
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.306
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4980
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.312
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.1067
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3228
_refine_ls_wR_factor_ref         0.3451
_reflns_number_gt                3506
_reflns_number_total             4980
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b903771c.txt
_cod_data_source_block           pat24_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_cell_volume        5487.8(15)
_cod_original_sg_symbol_H-M      I2/m
_cod_database_code               7053246