Non-cyclic formylated dipyrromethanes as phosphate anion receptors
Deliomeroglu, Murat K.; Lynch, Vincent M.; Sessler, Jonathan L.; Chem. Sci. 7 (2016) 3843–; doi:10.1039/C6SC00015K

data_1542552
_publ_section_title
;
 Non-cyclic formylated dipyrromethanes as phosphate anion receptors
;
_journal_issue                   6
_journal_name_full               'Chem. Sci.'
_journal_page_first              3843
_journal_paper_doi               10.1039/C6SC00015K
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety
'C30 H26 N4 O4, 2 C16 H36 N 1+, H2 P2 O7 2-, 1/2 C H2 Cl2'
_chemical_formula_sum            'C62.5 H99 Cl N6 O11 P2'
_chemical_formula_weight         1207.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-28 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
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_cell_angle_gamma                90
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.1
_cell_measurement_theta_min      3.49
_cell_volume                     6606.47(19)
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'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_collection
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_structure_solution
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Agilent SuperNova with AtlasS2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35854
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.239
_diffrn_reflns_theta_min         2.886
_diffrn_source                   'microfocus sealed tube'
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_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2604
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/n-pentane'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         13076
_refine_ls_number_restraints     535
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0827P)^2^+5.3705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10231
_reflns_number_total             13076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00015k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1542550--1542554.cif.'
_cod_original_formula_sum        'C62.50 H99 Cl N6 O11 P2'
_cod_database_code               1542552
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_estimated_absorpt_t_min   0.800
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              89695
_shelx_hkl_checksum              11630
_shelx_fab_checksum              28847