1-Pyrenyl- and 3-Perylenyl-antimony(V) Derivatives for the Fluorescence Turn-On Sensing of Fluoride Ions in Water at Sub-ppm Concentrations
Hirai, Masato; Myahkostupov, Mykhaylo; Castellano, Felix N.; Gabbaï, François P.; Organometallics 35 (2016) 1854–; doi:10.1021/acs.organomet.6b00233

data_4088608
_publ_section_title
;
 1-Pyrenyl- and 3-Perylenyl-antimony(V) Derivatives for the Fluorescence
 Turn-On Sensing of Fluoride Ions in Water at Sub-ppm Concentrations
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1854
_journal_paper_doi               10.1021/acs.organomet.6b00233
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C38 H26 Br Sb'
_chemical_formula_sum            'C38 H26 Br Sb'
_chemical_formula_weight         684.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 114.509(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.230(4)
_cell_length_b                   11.474(3)
_cell_length_c                   16.730(4)
_cell_measurement_reflns_used    9484
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.84
_cell_measurement_theta_min      2.16
_cell_volume                     3184.1(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36102
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.314
_diffrn_reflns_theta_min         1.775
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       needle
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
; 
 Flack x determined using 4862 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.714
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         14271
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.714
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0907P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                11638
_reflns_number_total             14271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00233_si_002.cif
_cod_data_source_block           3Br
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'none' was changed to '?'
-- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C76 H52 Br2 Sb2'
_cod_original_formula_weight         1368.49
_cod_original_formula_moiety         '2(C38 H26 Br Sb)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3184.2(13)
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4088608
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.768
_shelx_estimated_absorpt_t_max   0.847
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              65025
_shelx_hkl_checksum              51653
_shelx_fab_checksum              42331