Layered Calcium Structures of p-Phosphonic Acid O-Methyl-Calix[6]arene.
Clark, Thomas E.; Martin, Adam; Makha, Mohamed; Sobolev, Alexandre N.; Su, Dian; Rohrs, Henry W.; Gross, Michael L.; Raston, Colin L.; Crystal growth & design 10 (2010) 3211–3217; doi:10.1021/cg1003484

data_4501742
_publ_section_title
;
 Layered Calcium Structures of p-Phosphonic Acid O-Methyl-Calix[6]arene.
;
_journal_issue                   7
_journal_name_full               'Crystal growth &amp; design'
_journal_page_first              3211
_journal_page_last               3217
_journal_paper_doi               10.1021/cg1003484
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C48 H46 O24 P6, Ca4, 26.5(H2 O)'
_chemical_formula_sum            'C48 H99 Ca4 O50.5 P6'
_chemical_formula_weight         1830.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                112.047(7)
_cell_angle_beta                 95.814(5)
_cell_angle_gamma                108.467(6)
_cell_formula_units_Z            1
_cell_length_a                   11.4113(7)
_cell_length_b                   12.9903(9)
_cell_length_c                   15.4684(11)
_cell_measurement_reflns_used    3480
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.1
_cell_measurement_theta_min      3.12
_cell_volume                     1951.6(3)
_computing_cell_refinement
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_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 10.4738
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_sigmaI/netI    0.1485
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22732
_diffrn_reflns_theta_full        67.30
_diffrn_reflns_theta_max         67.30
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    4.520
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             961
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                3372
_reflns_number_total             6828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1003484_si_004.cif
_cod_data_source_block           Complex5c
_cod_depositor_comments
;
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_original_cell_volume        1951.6(2)
_cod_original_formula_sum        'C48 H99 Ca4 O50.50 P6'
_cod_database_code               4501742