Direct organocatalytic stereoselective transfer hydrogenation of conjugated olefins of steroids
Ramachary, Dhevalapally B.; Sakthidevi, Rajasekar; Reddy, P. Srinivasa; RSC Advances 3 (2013) 13497–; doi:10.1039/c3ra41519h

data_7239052
_publ_section_title
;
 Direct organocatalytic stereoselective transfer hydrogenation of
 conjugated olefins of steroids
;
_journal_issue                   32
_journal_name_full               'RSC Advances'
_journal_page_first              13497
_journal_paper_doi               10.1039/c3ra41519h
_journal_volume                  3
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_formula_sum            'C20 H30 O3'
_chemical_formula_weight         318.44
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.77744(12)
_cell_length_b                   14.0740(3)
_cell_length_c                   19.0348(4)
_cell_measurement_reflns_used    3402
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.9145
_cell_measurement_theta_min      3.1374
_cell_volume                     1815.65(6)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program.
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program.
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)/Bruker'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3291
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
1 omega 17.00 65.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 37.0000 -180.0000 48
2 omega -76.00 21.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 0.0000 -150.0000 97
3 omega -107.00 -81.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 179.0000 -180.0000 26
4 omega -8.00 18.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 55.1592 -77.0000 120.0000 26
5 omega -1.00 25.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 55.1592 -37.0000 -60.0000 26
6 omega 41.00 78.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 55.1592 -77.0000 120.0000 37
7 omega 90.00 116.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 110.3184 -50.0000 -30.0000 26
8 omega 82.00 143.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 110.3184 -25.0000 30.0000 61
9 omega 90.00 132.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 110.3184 -50.0000 0.0000 42
10 omega 87.00 125.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 110.3184 -50.0000 150.0000 38
11 omega 82.00 118.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 110.3184 -25.0000 -180.0000 36
12 omega 47.00 93.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 110.3184 -95.0000 -143.0000 46
13 omega 127.00 174.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 110.3184 111.0000 -60.0000 47
14 omega 82.00 107.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 110.3184 -25.0000 90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0413634
_diffrn_orient_matrix_UB_12      0.1076944
_diffrn_orient_matrix_UB_13      0.0015617
_diffrn_orient_matrix_UB_21      -0.084332
_diffrn_orient_matrix_UB_22      -0.0093199
_diffrn_orient_matrix_UB_23      0.0749638
_diffrn_orient_matrix_UB_31      0.206708
_diffrn_orient_matrix_UB_32      0.0176088
_diffrn_orient_matrix_UB_33      0.0305966
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0072
_diffrn_reflns_av_sigmaI/netI    0.0092
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4323
_diffrn_reflns_theta_full        72.06
_diffrn_reflns_theta_max         72.06
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.8435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+0.0925P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                2627
_reflns_number_total             2870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41519h.txt
_cod_data_source_block           NABA
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1815.64(6)
_cod_database_code               7239052