Preparation of organic mechanochromic fluorophores with simple structures and promising mechanochromic luminescence properties
Li, Gaocan; Xu, Yangyang; Zhuang, Weihua; Wang, Yunbing; RSC Adv.  (2016) –; doi:10.1039/C6RA20022B

data_7226443
_publ_section_title
;
 Preparation of organic mechanochromic fluorophores with simple structures
 and promising mechanochromic luminescence properties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA20022B
_journal_year                    2016
_chemical_formula_moiety         'C29 H38 P, F6 P'
_chemical_formula_sum            'C29 H38 F6 P2'
_chemical_formula_weight         562.53
_chemical_name_systematic        '1 PF6'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-07 deposited with the CCDC.
2016-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                107.945(4)
_cell_angle_beta                 96.334(4)
_cell_angle_gamma                107.336(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7112(6)
_cell_length_b                   11.0294(6)
_cell_length_c                   13.6960(5)
_cell_measurement_reflns_used    3613
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5140
_cell_measurement_theta_min      3.7180
_cell_volume                     1432.52(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXH-1997 (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -65.00  -39.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669 -178.0000   60.0000 26

  2 omega  -42.00   52.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669   77.0000 -150.0000 94

  3 omega  -70.00  -45.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669 -178.0000 -120.0000 25

  4 omega  -80.00   12.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -77.0000   90.0000 92

  5 omega  -11.00   18.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -99.0000  -30.0000 29

  6 omega   -1.00   69.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       16.6856   38.0000    0.0000 70

  7 omega   50.00   84.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       16.6856   57.0000    0.0000 34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0446522000
_diffrn_orient_matrix_UB_12      -0.0530390000
_diffrn_orient_matrix_UB_13      0.0115627000
_diffrn_orient_matrix_UB_21      -0.0109168000
_diffrn_orient_matrix_UB_22      -0.0449564000
_diffrn_orient_matrix_UB_23      -0.0524578000
_diffrn_orient_matrix_UB_31      0.0543159000
_diffrn_orient_matrix_UB_32      -0.0194347000
_diffrn_orient_matrix_UB_33      0.0152433000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11380
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1104P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1793
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                3795
_reflns_number_total             5842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra20022b2.cif
_cod_data_source_block           151022_s1_lgs_m
_cod_original_cell_volume        1432.53(12)
_cod_database_code               7226443
_reflns_odcompleteness_completeness 99.78
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F4) = Uanis(F4A)
Uanis(F3) = Uanis(F3A)
Uanis(F6) = Uanis(F6A)
Uanis(F5) = Uanis(F5A)
3. Others
 Sof(F4A)=Sof(F3A)=Sof(F6A)=Sof(F5A)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C27(H27a,H27b), C19(H19a,H19b), C23(H23a,H23b), C24(H24a,
 H24b), C25(H25a,H25b), C28(H28a,H28b), C20(H20a,H20b), C21(H21a,H21b), C1(H1a,
 H1b)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C10(H10), C9(H9), C15(H15), C1AA(H1AA), C7(H7), C6(H6), C4(H4),
 C3(H3)
4.c Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C22(H22a,H22b,H22c), C2(H2a,H2b,H2c)
;
_olex2_submission_special_instructions 'No special instructions were received'