Design and Synthesis of Tridentate Facially Chelating Ligands of the [2.n.1]-(2,6)-Pyridinophane Family
Andrei N. Vedernikov; Maren Pink; Kenneth G. Caulton; Journal of Organic Chemistry 68 (2003) 4806–4814; doi:10.1021/jo034268v

data_4022427
_publ_section_title
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 Design and Synthesis of Tridentate Facially Chelating
 Ligands of the [2.n.1]-(2,6)-Pyridinophane Family
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_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4806
_journal_page_last               4814
_journal_paper_doi               10.1021/jo034268v
_journal_volume                  68
_journal_year                    2003
_chemical_formula_moiety         'C19 H19 N3, 2(s O3 C F3)'
_chemical_formula_sum            'C21 H19 F6 N3 O6 S2'
_chemical_formula_weight         587.51
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                67.7110(10)
_cell_angle_beta                 81.3130(10)
_cell_angle_gamma                83.9190(10)
_cell_formula_units_Z            2
_cell_length_a                   8.6423(3)
_cell_length_b                   10.9307(3)
_cell_length_c                   14.1882(4)
_cell_measurement_reflns_used    9187
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.39
_cell_volume                     1224.20(6)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker; XTEL, local library'
_computing_publication_material  'SHELXTL, Bruker; XTEL, local library'
_computing_structure_refinement  'SHELXL-97, Sheldrick (1997)'
_computing_structure_solution    'SIR-92, Altomare et al. (1992)'
_diffrn_ambient_temperature      112(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'0.30 degree frames measured for 20 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22491
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  815
_diffrn_standards_number         9188
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.9818
_exptl_absorpt_correction_T_min  0.9411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         7133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0454P)^2^+0.8430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                5181
_reflns_number_total             7133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo034268vsi20030303_024323_2.cif
_cod_data_source_block           01102m
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4022427