Organization of Lower RimO-Alkylatedp-Phosphonic Acid Calix[4]arenes
Clark, Thomas E.; Makha, Mohamed; Sobolev, Alexandre N.; Su, Dian; Rohrs, Henry; Gross, Michael L.; Raston, Colin L.; Crystal Growth & Design 9 (2009) 3575–; doi:10.1021/cg900315h

data_4509544
_publ_section_title
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 Organization of Lower RimO-Alkylatedp-Phosphonic Acid Calix[4]arenes
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3575
_journal_paper_doi               10.1021/cg900315h
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C116 H204 O16 P4, H2 O'
_chemical_formula_sum            'C116 H206 O17 P4'
_chemical_formula_weight         1996.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.47(2)
_cell_angle_beta                 90.39(2)
_cell_angle_gamma                94.84(2)
_cell_formula_units_Z            2
_cell_length_a                   12.105(4)
_cell_length_b                   12.533(3)
_cell_length_c                   39.051(5)
_cell_measurement_reflns_used    4297
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.55
_cell_volume                     5852(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.6 (release 02-03-2006 CrysAlis171 .NET)
(compiled Mar  2 2006,16:42:47)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.6 (release 02-03-2006 CrysAlis171 .NET)
(compiled Mar  2 2006,16:42:47)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.6 (release 02-03-2006 CrysAlis171 .NET)
(compiled Mar  2 2006,16:42:47)
;
_computing_molecular_graphics    'X-Seed 2.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.447
_diffrn_measured_fraction_theta_max 0.447
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur-S, Sapphire CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1352
_diffrn_reflns_av_sigmaI/netI    0.1801
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            30697
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.11806
_exptl_absorpt_correction_T_min  0.89044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.6 (release 02-03-2006 CrysAlis171 .NET)
(compiled Mar  2 2006,16:42:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         9230
_refine_ls_number_restraints     668
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.2850
_refine_ls_R_factor_gt           0.1954
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+121.0769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4051
_refine_ls_wR_factor_ref         0.4539
_reflns_number_gt                5276
_reflns_number_total             9230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900315hsup1.cif
_cod_data_source_block           717636
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4509544