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_4029770
_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         'C28 H35 N8 O5, C H4 O, Cl'
_chemical_formula_sum            'C29 H39 Cl N8 O6'
_chemical_formula_weight         631.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 106.6480(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4965(2)
_cell_length_b                   13.0048(2)
_cell_length_c                   18.7848(3)
_cell_measurement_reflns_used    6541
_cell_measurement_temperature    123
_cell_measurement_theta_max      66.3576
_cell_measurement_theta_min      2.4488
_cell_volume                     2924.84(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 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 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega  -86.00  -33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000  150.0000    0.0000    0.0000 53

  2 omega   12.00   53.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -98.0000  240.0000    0.0000    0.0000 41

  3 omega  -14.00   33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137   45.0000    0.0000    0.0000    0.0000 47

  4 omega  -83.00  -36.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000   30.0000    0.0000    0.0000 47

  5 omega -111.00  -57.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   98.0000  299.0000    0.0000    0.0000 54

  6 omega -115.00  -61.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  109.0000  210.0000    0.0000    0.0000 54

  7 omega -173.00 -100.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -98.0000   12.0000    0.0000    0.0000 73

  8 omega -165.00  -62.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000   49.0000    0.0000    0.0000 103

  9 omega -124.00  -15.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   77.0000  120.0000    0.0000    0.0000 109

 10 omega   66.00  151.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  300.0000    0.0000    0.0000 85

 11 omega   72.00  119.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  229.0000    0.0000    0.0000 47

 12 omega   68.00  121.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  120.0000    0.0000    0.0000 53

;
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12699
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.47
_diffrn_reflns_theta_max         66.47
_diffrn_reflns_theta_min         3.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0586
_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^)+(0.1013P)^2^+2.3883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1742
_reflns_number_gt                3945
_reflns_number_total             4997
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            1860-5397-5-26-S2.cif
_cod_data_source_block           h127
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4029770