Synthetic Model of the Phosphate Binding Protein: Solid-State Structure and Solution-Phase Anion Binding Properties of a Large Oligopyrrolic Macrocycle
Evgeny A. Katayev; Jonathan L. Sessler; Victor N. Khrustalev; Yuri A. Ustynyuk; Journal of Organic Chemistry 72 (2007) 7244–7252; doi:10.1021/jo071106g

data_4024177
_publ_section_title
;
 Synthetic Model of the Phosphate Binding Protein: Solid-State
 Structure and Solution-Phase Anion Binding Properties of
 a Large Oligopyrrolic Macrocycle
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7244
_journal_page_last               7252
_journal_paper_doi               10.1021/jo071106g
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C111 H113 N21 O6 2+, H O4 P 2-'
_chemical_formula_sum            'C111 H114 N21 O10 P'
_chemical_formula_weight         1933.20
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.980(5)
_cell_angle_beta                 78.128(5)
_cell_angle_gamma                84.935(5)
_cell_formula_units_Z            4
_cell_length_a                   21.414(4)
_cell_length_b                   23.166(4)
_cell_length_c                   24.601(5)
_cell_measurement_reflns_used    5269
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      21.25
_cell_measurement_theta_min      2.25
_cell_volume                     11896(4)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL, v. 5.10 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL, v. 5.10 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL, v. 5.10 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL, v. 5.10 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      120.0(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0890
_diffrn_reflns_av_sigmaI/netI    0.3016
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            81706
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         0.85
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2311
_refine_ls_number_reflns         41388
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.2392
_refine_ls_R_factor_gt           0.0996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1837
_reflns_number_gt                12252
_reflns_number_total             41388
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo071106g-File001.cif
_cod_data_source_block           SA_H3PO4
_cod_depositor_comments
;
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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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               4024177