Synthesis of functionalised aromatic oligamide rods
Plante, Jeffrey; Campbell, Fred; Malkova, Barbora; Kilner, Colin; Warriner, Stuart L.; Wilson, Andrew J.; Organic & Biomolecular Chemistry 6 (2008) 138–146; doi:10.1039/b712606a

data_7150799
_publ_section_title
;
 Synthesis of functionalised aromatic oligamide rods
;
_journal_issue                   1
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              138
_journal_page_last               146
_journal_paper_doi               10.1039/b712606a
_journal_volume                  6
_journal_year                    2008
_chemical_compound_source        Synthesized
_chemical_formula_moiety         'C35 H35 N3 O9'
_chemical_formula_sum            'C35 H35 N3 O9'
_chemical_formula_weight         641.66
_chemical_name_common            Nitro-Bn-iPr-nPr-Ester
_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                105.2700(10)
_cell_angle_beta                 98.0820(10)
_cell_angle_gamma                98.0750(10)
_cell_formula_units_Z            2
_cell_length_a                   8.0680(2)
_cell_length_b                   10.8740(2)
_cell_length_c                   19.1980(5)
_cell_measurement_reflns_used    7022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.00
_cell_volume                     1580.65(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 2004)'
_computing_data_reduction
;
DENZO-SMN and COLLECT (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_publication_material
;
enCIFer: A program for viewing, editing and visualising CIFs.
F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler,
J. Applied Cryst., 37, 331-334, 2004
;
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, 1997)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_structure_solution
;
SIR92
Altomare, A.; Burla, M. C.; Camalli, G.; Cascarano, G.;
Giacovazzo, C.; Guagliardi, A.; Polidori, G.
J. Appl. Cryst. 1994, 27, 435-436.
SHELXS-97 (Sheldrick, 1997)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type
;
Nonius KappaCCD area-detector diffractometer
;
_diffrn_measurement_method
;
phi and omega scans to fill the asymmetric unit
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13724
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.97
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              Kappa
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             676
_exptl_crystal_recrystallization_method 'Slow Evaporation Ethyl Acetate'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0945P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                4799
_reflns_number_total             7244
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712606a.txt
_cod_data_source_block           NitroPheIleLeuEster
_cod_original_cell_volume        1580.64(6)
_cod_database_code               7150799