Novel retinylidene iminium salts for defining opsin shifts: synthesis and intrinsic chromophoric properties.
Petersen, Michael Axman; Nielsen, Iben B.; Kristensen, Michael B.; Kadziola, Anders; Lammich, Lutz; Andersen, Lars H.; Nielsen, Mogens Brøndsted; Organic & biomolecular chemistry 4 (2006) 1546–1554; doi:10.1039/b600121a

data_7150436
_publ_section_title
;
 Novel retinylidene iminium salts for defining opsin shifts: synthesis
 and intrinsic chromophoric properties.
;
_journal_issue                   8
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1546
_journal_page_last               1554
_journal_paper_doi               10.1039/b600121a
_journal_volume                  4
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_formula_sum            'C22 H29 N'
_chemical_formula_weight         307.46
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus/SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   9.8070(8)
_cell_length_b                   11.7490(12)
_cell_length_c                   16.027(2)
_cell_measurement_reflns_used    29983
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      35.01
_cell_measurement_theta_min      2.15
_cell_volume                     1846.7(3)
_computing_cell_refinement       'COLLECT (Nonius, 1999)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      122(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  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52673
_diffrn_reflns_theta_full        35.01
_diffrn_reflns_theta_max         35.01
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         8043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0485P)^2^+0.2961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                7116
_reflns_number_total             8043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b600121a.txt
_cod_data_source_block           shelxl
_cod_original_cell_volume        1846.7(4)
_cod_database_code               7150436