Isolation and structural determination of non-racemic tertiary cathinone derivatives.
Zhou, M.-J.; Bouazzaoui, S.; Jones, L. E.; Goodrich, P.; Bell, S. E. J.; Sheldrake, G. N.; Horton, P. N.; Coles, S. J.; Fletcher, N. C.; Organic & biomolecular chemistry 13 (2015) 9629–9636; doi:10.1039/c5ob01306b

data_7154630
_publ_section_title
;
 Isolation and structural determination of non-racemic tertiary cathinone
 derivatives.
;
_journal_issue                   37
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9629
_journal_page_last               9636
_journal_paper_doi               10.1039/c5ob01306b
_journal_volume                  13
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C20 H17 O8, C11 H16 N O'
_chemical_formula_sum            'C31 H33 N O9'
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_space_group_name_H-M_alt        'P 1 21 1'
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_atom_sites_solution_hydrogens   geom
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_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_formula_units_Z            2
_cell_length_a                   8.2681(5)
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_cell_measurement_reflns_used    12666
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
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_cell_volume                     1454.40(17)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
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_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
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_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_unetI/netI     0.1207
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
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_diffrn_reflns_limit_k_min       -9
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_diffrn_reflns_limit_l_min       -30
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_diffrn_reflns_point_group_measured_fraction_full 0.972
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_diffrn_source                   'Rotating Anode'
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       Plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 1042 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.6(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6380
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.0865
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+0.4153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2310
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                3708
_reflns_number_total             6380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob01306b2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7154630.cif.
;
_cod_database_code               7154630
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              67508