Hydrogen-bonding cyclodiphosphazanes: superior effects of 3,5-(CF3)2-substitution in anion-recognition and counter-ion catalysis
Wolf, Florian F.; Neudörfl, Jörg-M.; Goldfuss, Bernd; New Journal of Chemistry 42 (2018) 4854–; doi:10.1039/C7NJ04660J

data_7056997
_publ_section_title
;
 Hydrogen-bonding cyclodiphosphazanes: superior effects of
 3,5-(CF3)2-substitution in anion-recognition and counter-ion catalysis
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4854
_journal_paper_doi               10.1039/C7NJ04660J
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C28 H36 F12 N4 O4 P2 S'
_chemical_formula_weight         814.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-14 deposited with the CCDC.
2018-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0313(4)
_cell_length_b                   21.6500(6)
_cell_length_c                   12.1766(3)
_cell_measurement_temperature    100(2)
_cell_volume                     3698.98(17)
_computing_cell_refinement       'Bruker APEX 3'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'Bruker APEX 3'
_computing_molecular_graphics    'SCHAKAL99 (E. Keller 1999)'
_computing_publication_material  'PLATON (A. L. Spek 1980-2015)'
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2014)
SHELXLE (C. B. Huebschle 2016)'
;
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       'phi / omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26645
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        66.792
_diffrn_reflns_theta_max         66.792
_diffrn_reflns_theta_min         3.754
_diffrn_source                   'micro focus'
_exptl_absorpt_coefficient_mu    2.504
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 2671 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.046(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6394
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0704P)^2^+3.2729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                6172
_reflns_number_total             6394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj04660j2.cif
_cod_data_source_block           fwfr11
_cod_depositor_comments
'Adding full bibliography for 7056994--7056999.cif.'
_cod_database_code               7056997
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.520
_shelx_estimated_absorpt_t_max   0.705
_shelx_res_checksum              87614