Colorimetric and Luminescent Sensors for Chloride: Hydrogen Bonding vs Deprotonation
Elmes, Robert B. P.; Turner, Peter; Jolliffe, Katrina A.; Organic Letters 15 (2013) 5638–; doi:10.1021/ol402500q

data_1513108
_publ_section_title
;
 Colorimetric and Luminescent Sensors for Chloride: Hydrogen Bonding vs
 Deprotonation
;
_journal_issue                   22
_journal_name_full               'Organic Letters'
_journal_page_first              5638
_journal_paper_doi               10.1021/ol402500q
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C41 H54 Cl N3 O2'
_chemical_formula_weight         656.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_method           SHELXL-97
_cell_angle_alpha                64.761(7)
_cell_angle_beta                 82.738(11)
_cell_angle_gamma                79.399(9)
_cell_formula_units_Z            4
_cell_length_a                   8.677(3)
_cell_length_b                   21.099(10)
_cell_length_c                   22.462(10)
_cell_measurement_reflns_used    9692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.45
_cell_volume                     3651(3)
_computing_cell_refinement       'SAINT (Bruker-AXS,2012)'
_computing_data_collection       'APEX (Bruker-AXS,2012)'
_computing_data_reduction        'SAINT and XPREP (Bruker-AXS,2012)'
_computing_molecular_graphics
;
  xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999)
  ORTEPII  (Johnson,C.K., 1976). 
  WinGX (Farrugia, 1999)
  shelXle (H&#x00FC;bschle,C.B., et al., 2011)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N, to a short length 
of fibre supported on a thin piece of copper wire 
inserted in a copper mounting pin.  The crystal was 
quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            107219
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.7945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.555
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         19583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.555
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+0.5P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                15109
_reflns_number_total             19583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol402500q_si_002.cif
_cod_data_source_block           4.TBACl_kaj12pt3
_cod_database_code               1513108