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_4321464
_publ_section_title
;
 Main-Group-Element Calix[4]arenes: Variable Coordination and
 Conformational Isomerism at Phosphorus and Silicon
;
_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            'C53 H71 O6 P'
_chemical_formula_weight         835.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   44.267(4)
_cell_length_b                   44.267(4)
_cell_length_c                   13.311(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    228(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     22589(3)
_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      228(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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4912
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         1.84
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.100
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       rod-liked
_exptl_crystal_F_000             8136
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00081(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         3946
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.268
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_obs          0.1012
_refine_ls_shift/esd_max         -0.028
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1796P)^2^+154.4351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3669
_refine_ls_wR_factor_obs         0.2562
_reflns_number_observed          2952
_reflns_number_total             4538
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000349n_3.cif
_cod_data_source_block           hv-p698_IC000349N_structure_11a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1796P)^2^+154.4351P] 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^)+(0.1796P)^2^+154.4351P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        '[C45 H55 O4 P] . 2[C4 H8 O]'
_cod_database_code               4321464