Variations in the solid-state, solution and theoretical structures of a laterally deprotonated aromatic tertiary amide
Andrew Wheatley; David R. Armstrong; Jonathan Clayden; Robert Haigh; David J. Linton; Paul Schooler; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b302283h

data_7103737
_publ_section_title
;
Variations in the solid-state, solution and
theoretical structures of a laterally deprotonated aromatic tertiary
amide
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b302283h
_journal_year                    2003
_chemical_formula_sum            'C31 H48.5 Li N O4'
_chemical_formula_weight         506.15
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.384(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9696(4)
_cell_length_b                   18.6529(8)
_cell_length_c                   16.5704(5)
_cell_measurement_reflns_used    14076
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1
_cell_volume                     3078.8(2)
_computing_cell_refinement
;
HKL Scalepack (Otwinowski & Minor, 1997) 
;
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo & Scalepack (Otwinowski, 1997) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17732
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9841
_exptl_absorpt_correction_T_min  0.9759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sortav-Blessing, 1995
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.7(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         8977
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.180
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1124P)^2^+1.1333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.2004
_reflns_number_gt                7273
_reflns_number_total             8977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302283h.txt
_cod_data_source_block           s92
_cod_original_sg_symbol_H-M      'P n'
_cod_original_formula_sum        'C31 H48.50 Li N O4'
_cod_database_code               7103737