Main-Group-Element Calix[4]arenes: Variable Coordination and Conformational Isomerism at Phosphorus and Silicon
Maomian Fan; Igor V. Shevchenko; R. Harmony Voorhies; Scott F. Eckert; Hongming Zhang; Michael Lattman; Inorganic Chemistry 39 (2000) 4704–4712; doi:10.1021/ic000349n

data_4321463
_publ_section_title
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 Main-Group-Element Calix[4]arenes: Variable Coordination and
 Conformational Isomerism at Phosphorus and Silicon
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4704
_journal_page_last               4712
_journal_paper_doi               10.1021/ic000349n
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C50 H71 I6 O4 P'
_chemical_formula_weight         1528.44
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 104.18(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.328(2)
_cell_length_b                   21.560(4)
_cell_length_c                   20.720(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     5772.5(18)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'SHELXL-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7193
_diffrn_reflns_theta_max         22.01
_diffrn_reflns_theta_min         1.84
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.294
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   '\y scan'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_description       plates
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.766
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6188
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_obs          0.0681
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+70.3142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1971
_refine_ls_wR_factor_obs         0.1641
_reflns_number_observed          4749
_reflns_number_total             6841
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000349n_2.cif
_cod_data_source_block           is-pmei_IC000349_structure_10a(I)
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+70.3142P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+70.3142P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5773(2)
_cod_database_code               4321463