Spiro Tröger's base derivatives: another structural phoenix?
Tatar, Ameneh; Cejka, Jan; Král, Vladimír; Dolenský, Bohumil; Organic letters 12 (2010) 1872–1875; doi:10.1021/ol1004774

data_1502936
_publ_section_title
;
 Spiro Tr\"oger's base derivatives: another structural phoenix?
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1872
_journal_page_last               1875
_journal_paper_doi               10.1021/ol1004774
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C27 H22 N2 O4'
_chemical_formula_sum            'C27 H22 N2 O4'
_chemical_formula_weight         438.48
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 107.201(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4584(9)
_cell_length_b                   12.4190(7)
_cell_length_c                   12.0130(8)
_cell_measurement_reflns_used    6124
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      4
_cell_volume                     2060.6(2)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.1917
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_orient_matrix_UB_11      -0.0007147764
_diffrn_orient_matrix_UB_12      -0.0306578352
_diffrn_orient_matrix_UB_13      -0.1033634248
_diffrn_orient_matrix_UB_21      0.0110809479
_diffrn_orient_matrix_UB_22      0.1197997182
_diffrn_orient_matrix_UB_23      -0.0235927750
_diffrn_orient_matrix_UB_31      0.1338197562
_diffrn_orient_matrix_UB_32      -0.0101169638
_diffrn_orient_matrix_UB_33      0.0344845084
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17332
_diffrn_reflns_theta_full        71.958
_diffrn_reflns_theta_max         78.215
_diffrn_reflns_theta_min         4.788
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9452
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000160
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.16P)^2^ + 0.20P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1997
_refine_ls_wR_factor_gt          0.1805
_refine_ls_wR_factor_ref         0.1997
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3198
_reflns_number_total             4285
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_r_factor_ref   0.0806
_oxford_refine_ls_scale          3.42(9)
_oxford_reflns_number_all        4285
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ol1004774_si_002.cif
_cod_data_source_block           AT_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               1502936