9-Iodophenalenone and 9-trifluoromethanesulfonyloxyphenalenone: convenient entry points to new phenalenones functionalised at the 9-position. Iodine-carbonyl interaction studies by X-ray crystallography
Anamimoghadam, Ommid; Long, De-Liang; Bucher, Götz; RSC Adv. 4 (2014) 56654–; doi:10.1039/C4RA00178H

data_7218653
_publ_section_title
;
 9-Iodophenalenone and 9-trifluoromethanesulfonyloxyphenalenone:
 convenient entry points to new phenalenones functionalised at the
 9-position. Iodine-carbonyl interaction studies by X-ray crystallography
;
_journal_issue                   100
_journal_name_full               'RSC Adv.'
_journal_page_first              56654
_journal_paper_doi               10.1039/C4RA00178H
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C20.5 H15 F3 N O4.5 S'
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_symmetry_space_group_name_H-M   'P 21 21 21'
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_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.00
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_cell_length_a                   23.961(5)
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_cell_measurement_temperature    150(2)
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_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
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_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker ApexII Quasar CCD'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.229
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_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
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_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.35
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(17)
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         6873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.2125
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                3094
_reflns_number_total             6873
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4ra00178h2.cif
_cod_data_source_block           oa157
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 2827 2014-09-09 07:05:25Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3832.3(14)
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C20.50 H15 F3 N O4.50 S'
_cod_database_code               7218653