Chiral transmission to crystal photodimerizations of leucine–methionine quasiracemic assemblies
Lu, Yuhua; Bolokowicz, Andrew. J.; Reeb, Sarah A.; Wiseman, Joshua D.; Wheeler, Kraig A.; RSC Advances 4 (2014) 8125–; doi:10.1039/c3ra47270a

data_7235318
_publ_section_title
;
 Chiral transmission to crystal photodimerizations of leucine--methionine
 quasiracemic assemblies
;
_journal_issue                   16
_journal_name_full               'RSC Advances'
_journal_page_first              8125
_journal_paper_doi               10.1039/c3ra47270a
_journal_volume                  4
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C29 H36 N2 O12 S3'
_chemical_formula_sum            'C29 H36 N2 O12 S3'
_chemical_formula_weight         700.78
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.437(5)
_cell_angle_beta                 98.844(5)
_cell_angle_gamma                99.960(5)
_cell_formula_units_Z            1
_cell_length_a                   6.8789(6)
_cell_length_b                   8.1405(7)
_cell_length_c                   14.5005(13)
_cell_measurement_reflns_used    8331
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      65.077
_cell_measurement_theta_min      2.812
_cell_volume                     788.25(12)
_computing_cell_refinement       APEX2
_computing_data_reduction
;
SAINT (Bruker, 2009) and XPREP (Bruker, 2009)
;
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24878
_diffrn_reflns_point_group_measured_fraction_full 0.469
_diffrn_reflns_point_group_measured_fraction_max 0.470
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.553
_diffrn_reflns_theta_min         3.092
_exptl_absorpt_coefficient_mu    2.732
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2010)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         2680
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1587P)^2^+0.2856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2113
_reflns_number_gt                2263
_reflns_number_total             2680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra47270a.cif
_cod_data_source_block           kaw111b_twin4
_cod_database_code               7235318
_shelxl_version_number           2013-4
_shelx_res_checksum              12737
_shelx_hkl_checksum              92518