Effect of anions on the solid-state interplay of symmetric and unsymmetric phosphonium cations
Ling, Irene; Skelton, Brian W.; Sobolev, Alexandre N.; Alias, Yatimah; Khor, Zong Chin; Raston, Colin L.; New Journal of Chemistry 44 (2020) 10220–10228; doi:10.1039/D0NJ01975E

data_7059670
_publ_section_title
;
 Effect of anions on the solid-state interplay of symmetric and
 unsymmetric phosphonium cations
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10220
_journal_page_last               10228
_journal_paper_doi               10.1039/D0NJ01975E
_journal_volume                  44
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H22 P, C2 F6 N O4 S2'
_chemical_formula_sum            'C27 H22 F6 N O4 P S2'
_chemical_formula_weight         633.54
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-12-02 deposited with the CCDC.	2020-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7732(6)
_cell_length_b                   8.4372(2)
_cell_length_c                   16.5014(14)
_cell_measurement_reflns_used    13213
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5426
_cell_measurement_theta_min      3.595
_cell_volume                     2752.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2015/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0225087589
_diffrn_orient_matrix_UB_12      -0.0367615962
_diffrn_orient_matrix_UB_13      0.0158117813
_diffrn_orient_matrix_UB_21      0.0190861144
_diffrn_orient_matrix_UB_22      -0.0167506571
_diffrn_orient_matrix_UB_23      -0.031953415
_diffrn_orient_matrix_UB_31      0.0785428545
_diffrn_orient_matrix_UB_32      0.0146106225
_diffrn_orient_matrix_UB_33      0.0032622916
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31268
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        32.000
_diffrn_reflns_theta_max         32.653
_diffrn_reflns_theta_min         3.604
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
       CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       rod
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2769 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         9173
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0291P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                7256
_reflns_number_total             9173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01975e1.cif
_cod_data_source_block           110301f
_cod_depositor_comments
;Adding full bibliography for 7059666--7059672.cif.

 Adding full bibliography for 7059666--7059672.cif.
;
_cod_database_code               7059670
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.875
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              99021