Tetrahedral Tetraphosphonic Acids. New Building Blocks in Supramolecular Chemistry
Schütrumpf, Alexandra; Kirpi, Erdoğan; Bulut, Aysun; Morel, Flavien L.; Ranocchiari, Marco; Lork, Enno; Zorlu, Yunus; Grabowsky, Simon; Yücesan, Gündoğ; Beckmann, Jens; Crystal Growth & Design 15 (2015) 4925–; doi:10.1021/acs.cgd.5b00811

data_4513551
_publ_section_title
;
 Tetrahedral Tetraphosphonic Acids. New Building Blocks in Supramolecular
 Chemistry
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4925
_journal_paper_doi               10.1021/acs.cgd.5b00811
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C105 H24 O32 P4'
_chemical_formula_sum            'C105 H24 O32 P4'
_chemical_formula_weight         640.32
_chemical_name_common            TPPA
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.197(3)
_cell_length_b                   13.197(3)
_cell_length_c                   7.5613(19)
_cell_measurement_reflns_used    1649
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      26.0897
_cell_measurement_theta_min      3.0871
_cell_volume                     1316.9(5)
_computing_cell_refinement       'APEX2 v2014.9-0 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service v2013.12.0.0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material
'PLATON V1.16 (Spek, 2009), SHELXTL V6.14 (Bruker AXS)'
_computing_structure_refinement  'SHELXTL V6.14 (Bruker AXS)'
_computing_structure_solution    'SHELXTL V6.14 (Bruker AXS)'
_diffrn_ambient_temperature      173.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker APEX II QUAZAR three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer QUAZAR mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3532
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         2.18
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              ImuS
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.309
_refine_ls_abs_structure_details
;
Flack x determined using 471 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.47(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1333
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                1217
_reflns_number_total             1333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b00811_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4513551--4513553.cif.'
_cod_original_cell_volume        1316.9(6)
_cod_database_code               4513551