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_4321465
_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            'C29 H24 O4 Si'
_chemical_formula_weight         464.57
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.88(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.751(3)
_cell_length_b                   17.892(5)
_cell_length_c                   11.774(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2198.7(11)
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4548
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.11
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.143
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       rod-liked
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.942
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0036(10)
_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   1.041
_refine_ls_goodness_of_fit_obs   1.130
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3894
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.115
_refine_ls_restrained_S_obs      1.138
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_obs          0.0774
_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^)+(0.0603P)^2^+5.4183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2060
_refine_ls_wR_factor_obs         0.1668
_reflns_number_observed          2796
_reflns_number_total             4316
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000349n_4.cif
_cod_data_source_block           mf-si04_IC000349N_structure_2b-c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+5.4183P] 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^)+(0.0603P)^2^+5.4183P] 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        2199(1)
_cod_database_code               4321465