An expedient, stereoselective synthesis of highly functionalized cyclic compounds
Ewa Krawczyk; Krzysztof Owsianik; Aleksandra Skowrońska; Michał Wieczorek; Wiesław Majzner; New J. Chem. 26 (2002) 1753–1767; doi:10.1039/b207700k

data_7051005
_publ_section_title
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 An expedient, stereoselective synthesis of highly functionalized
 cyclic compounds
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1753
_journal_page_last               1767
_journal_paper_doi               10.1039/b207700k
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         'C20 H37 O6 P S'
_chemical_formula_sum            'C20 H37 O6 P S'
_chemical_formula_weight         436.53
_chemical_name_common
;
Ethyl 1-[(dineopentoxyphosphoryl)sulfanyl]-3-
methyl-2-oxocyclohexanecarboxylate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.075(2)
_cell_length_b                   19.042(5)
_cell_length_c                   20.889(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      15.44
_cell_volume                     2416.4(14)
_computing_cell_refinement
;
Enraf--Nonius CAD-4 (Schagen, Straver, van Meurs & Williams, 1989)
;
_computing_data_collection
;
Enraf--Nonius CAD-4 (Schagen, Straver, van Meurs & Williams, 1989)
;
_computing_data_reduction
;
Enraf--Nonius SDP (Frenz, 1986; North, Phillips & Mathews, 1968)
;
_computing_molecular_graphics
;
SHELXTL-Plus - XP (Sheldrick, 1991)
;
_computing_publication_material
;
CSU (Vickovic, 1988)
;
_computing_structure_refinement
;
SHELXL-93 (Sheldrick, 1993)
;
_computing_structure_solution
;
SHELXS-86 (Sheldrick, 1990)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_sigmaI/netI    0.0828
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11162
_diffrn_reflns_theta_max         74.97
_diffrn_reflns_theta_min         3.14
_diffrn_standards_decay_%        15.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  0.9981
_exptl_absorpt_correction_T_min  0.9142
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(\y scans; North, Phillips, Mathews, 1968; Frenz, 1986)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1368
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                3385
_reflns_number_total             4976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207700k.txt
_cod_data_source_block           Compound9g
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_geom_bond_atom_site_label_D' replaced with
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'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
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'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
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'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_distance_DH' replaced with '_geom_hbond_distance_DH'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_HA' replaced with
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'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_DA' replaced with
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'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_angle_DHA' replaced with '_geom_hbond_angle_DHA' as
specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_site_symmetry_A' replaced with
'_geom_hbond_site_symmetry_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
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_cod_database_code               7051005