Easy wide scope access to luminescent fluorophosphoranes.
Ponce-de-León, Jaime; Infante, Rebeca; Espinet, Pablo; Chemical communications (Cambridge, England) 57 (2021) 5458–5461; doi:10.1039/d1cc00976a

data_7128257
_publ_section_title
;
 Easy wide scope access to luminescent fluorophosphoranes.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5458
_journal_page_last               5461
_journal_paper_doi               10.1039/d1cc00976a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C24 H22 F9 P'
_chemical_formula_sum            'C24 H22 F9 P'
_chemical_formula_weight         512.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-24 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.5949(5)
_cell_length_b                   17.1989(10)
_cell_length_c                   29.961(2)
_cell_measurement_reflns_used    2229
_cell_measurement_temperature    219.9(4)
_cell_measurement_theta_max      25.1980
_cell_measurement_theta_min      3.6010
_cell_volume                     4428.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      219.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -3.00  74.00   1.00   94.15    --   12.36  37.00-180.00   77
  2  \w    -10.00  24.00   1.00   94.15    --   12.36 -19.00   0.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0116954000
_diffrn_orient_matrix_UB_12      0.0149531000
_diffrn_orient_matrix_UB_13      0.0218167000
_diffrn_orient_matrix_UB_21      -0.0233590000
_diffrn_orient_matrix_UB_22      0.0361737000
_diffrn_orient_matrix_UB_23      -0.0091870000
_diffrn_orient_matrix_UB_31      -0.0782610000
_diffrn_orient_matrix_UB_32      -0.0129998000
_diffrn_orient_matrix_UB_33      -0.0005107000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12364
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.714
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             2096
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3'
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1505
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0949P)^2^+1.5579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2489
_reflns_number_total             5253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00976a2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7128255--7128257.cif.'
_cod_database_code               7128257
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C24 H22 F9 P'
_chemical_oxdiff_usercomment     'colorless plate'
_reflns_odcompleteness_completeness 98.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: H19(0.5) H19A(0.5) H24C(0.5) H24D(0.5) H24A(0.5) H24B(0.5)
 C21(0.5) H21A(0.5) H21B(0.5) C21A(0.5) H21C(0.5) H21D(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C19(H19), C19(H19A)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C14(H14A,H14B), C15(H15A,
 H15B), C20(H20A,H20B), C22(H22A,H22B), C24(H24C,H24D), C24(H24A,H24B),
 C21(H21A,H21B), C21A(H21C,H21D), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB)
;
_shelx_res_checksum              95582
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.776