Synthesis of rigidified flavin-guanidinium ion conjugates and investigation of their photocatalytic properties.
Schmaderer, Harald; Bhuyan, Mouchumi; König, Burkhard; Beilstein journal of organic chemistry 5 (2009) 26–; doi:10.3762/bjoc.5.26

data_4029762
_publ_section_title
;
 Synthesis of rigidified flavin-guanidinium ion conjugates and
 investigation of their photocatalytic properties.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              26
_journal_paper_doi               10.3762/bjoc.5.26
_journal_volume                  5
_journal_year                    2009
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C27 H31 N5 O6, C2 H6 O S'
_chemical_formula_sum            'C29 H37 N5 O7 S'
_chemical_formula_weight         599.71
_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
_cell_angle_alpha                84.158(4)
_cell_angle_beta                 81.210(4)
_cell_angle_gamma                71.668(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6278(4)
_cell_length_b                   11.8039(6)
_cell_length_c                   12.8185(5)
_cell_measurement_reflns_used    6440
_cell_measurement_temperature    123
_cell_measurement_theta_max      66.6659
_cell_measurement_theta_min      3.4871
_cell_volume                     1506.06(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega   33.00   86.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137   45.0000  180.0000    0.0000    0.0000 53

  2 omega   10.00   63.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   45.0000  120.0000    0.0000    0.0000 53

  3 omega  -36.00   21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -77.0000  180.0000    0.0000    0.0000 57

  4 omega   38.00   82.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137   45.0000  300.0000    0.0000    0.0000 44

  5 omega  -39.00   13.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   45.0000   90.0000    0.0000    0.0000 52

  6 omega  -86.00  -33.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000  330.0000    0.0000    0.0000 53

  7 omega -121.00  -58.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000  120.0000    0.0000    0.0000 63

  8 omega  -62.00   -1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000    0.0000    0.0000    0.0000 61

  9 omega -124.00  -65.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   77.0000    0.0000    0.0000    0.0000 59

 10 omega  -69.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   77.0000  210.0000    0.0000    0.0000 58

 11 omega -124.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   77.0000   90.0000    0.0000    0.0000 113

 12 omega -116.00  -82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  111.0000  265.0000    0.0000    0.0000 34

 13 omega -113.00  -63.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000  180.0000    0.0000    0.0000 50

 14 omega -113.00  -64.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  109.0000  152.0000    0.0000    0.0000 49

 15 omega -115.00  -64.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000   30.0000    0.0000    0.0000 51

 16 omega  -58.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   77.0000  120.0000    0.0000    0.0000 47

 17 omega  -96.00  -63.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  109.0000  357.0000    0.0000    0.0000 33

 18 omega   66.00  111.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  210.0000    0.0000    0.0000 45

 19 omega   66.00  115.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   30.0000    0.0000    0.0000 49

 20 omega   60.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000  330.0000    0.0000    0.0000 31

 21 omega   83.00  125.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000   30.0000    0.0000    0.0000 42

 22 omega   80.00  118.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   60.0000    0.0000    0.0000 38

 23 omega   66.00  113.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  330.0000    0.0000    0.0000 47

 24 omega   63.00  118.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000  270.0000    0.0000    0.0000 55

 25 omega   69.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  120.0000    0.0000    0.0000 58

 26 omega   20.00   50.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000 -132.0000  133.0000    0.0000    0.0000 30

 27 omega  118.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000   30.0000    0.0000    0.0000 34

 28 omega  116.00  160.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000  300.0000    0.0000    0.0000 44

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12218
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.67
_diffrn_reflns_theta_max         66.67
_diffrn_reflns_theta_min         3.49
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            parallelepiped
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1009P)^2^+1.5142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1888
_reflns_number_gt                4239
_reflns_number_total             5130
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            1860-5397-5-26-S3.cif
_cod_data_source_block           h215
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/Beilstein/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4029762