Substituted 2,4,4,6-tetraphenyl-4H-selenopyrans: preparation, photocolouration and 4H-selenopyran ring geometry; an X-ray and DFT calculation study
Jiří Kroulík; Jan Čejka; Stanislav Böhm; Pavel Šebek; Stanislav Nešp°urek; Igor Koshets; Petr Sedmera; Petr Halada; Vladimír Havlíček; Bohumil Kratochvíl; Josef Kuthan; J. Chem. Soc., Perkin Trans. 2  (2002) 1909–1916; doi:10.1039/b204976g

data_7204464
_publ_section_title
;
 Substituted 2,4,4,6-tetraphenyl-4H-selenopyrans: preparation,
 photocolouration and 4H-selenopyran ring geometry; an X-ray and DFT
 calculation study
;
_journal_issue                   11
_journal_name_full               'J. Chem. Soc., Perkin Trans. 2'
_journal_page_first              1909
_journal_page_last               1916
_journal_paper_doi               10.1039/b204976g
_journal_year                    2002
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C29 H20 Se1 '
_chemical_formula_sum            'C29 H20 Se'
_chemical_formula_weight         447.44
_chemical_melting_point          174.0(10)
_chemical_name_systematic
;                                                                               
2',6'-Diphenylspiro[fluorene-9.4'-selenopyran]                                                                               
;
_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
_audit_creation_date             02-28-04
_audit_creation_method           CRYSTALS_ver_28-04-02
_cell_angle_alpha                90
_cell_angle_beta                 90.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.862(3)
_cell_length_b                   14.597(3)
_cell_length_c                   27.479(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293
_cell_measurement_theta_max      40
_cell_measurement_theta_min      35
_cell_volume                     4356.4(16)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;                                                                               
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)                         
;
_computing_molecular_graphics
;                                                                               
CAMERON (Watkin, Prout & Pearce,  1996)                                        
;
_computing_publication_material
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_refinement
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '  Enraf-nonius CAD4 '
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11658
_diffrn_reflns_theta_max         55.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        2.18
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.41
_exptl_absorpt_correction_T_max  0.09
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '\y scan,(North et al, 1968)'
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             1820.66
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          1.00
_refine_diff_density_max         0.83
_refine_diff_density_min         -1.56
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0800
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         4485
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.000340
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 
21.7     24.0     21.0     8.40     1.47    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0790
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                4485
_reflns_number_total             5475
_reflns_threshold_expression     >1.96\s(I)
_cod_data_source_file            b204976g.txt
_cod_data_source_block           CRYSTALS_cif3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '173-175' was changed to '174.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        4356.4
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C29 H20 Se1 '
_cod_database_code               7204464