Acid/base controlled size modulation of capsular phosphates, hydroxide encapsulation, quantitative and clean extraction of sulfate with carbonate capsules of a tripodal urea receptor
Akhuli, Bidyut; Ravikumar, I.; Ghosh, Pradyut; Chemical Science 3 (2012) 1522–; doi:10.1039/c2sc00021k

data_1515234
_publ_section_title
;
 Acid/base controlled size modulation of capsular phosphates, hydroxide
 encapsulation, quantitative and clean extraction of sulfate with
 carbonate capsules of a tripodal urea receptor
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1522
_journal_paper_doi               10.1039/c2sc00021k
_journal_volume                  3
_journal_year                    2012
_chemical_formula_sum            'C86 H109 F30 N16 O10 P'
_chemical_formula_weight         2127.86
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.210(4)
_cell_length_b                   20.782(4)
_cell_length_c                   25.120(5)
_cell_measurement_temperature    100(2)
_cell_volume                     10028(3)
_computing_cell_refinement       'BRUKER SMART APEX II'
_computing_data_collection       'BRUKER SMART APEX II'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_molecular_graphics    PLATON
_computing_publication_material  'MERCURY 2.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD AREA DETECTOR'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28347
_diffrn_reflns_theta_full        21.05
_diffrn_reflns_theta_max         21.05
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_correction_T_min  0.9494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             4408
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(16)
_refine_ls_extinction_coef       0.00000(11)
_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_ref   1.482
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1289
_refine_ls_number_reflns         10636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.482
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          3.785
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                8855
_reflns_number_total             10636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc00021k.txt
_cod_data_source_block           test3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'ORTHORHOMBIC' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        10029(3)
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               1515234