What is your actual catalyst? TMS cleavage rates of diarylprolinol silyl ethers studied by in situ NMR
Haindl, Michael H.; Schmid, Markus B.; Zeitler, Kirsten; Gschwind, Ruth M.; RSC Advances 2 (2012) 5941–; doi:10.1039/c2ra20860a

data_7238686
_publ_section_title
;
 What is your actual catalyst? TMS cleavage rates of diarylprolinol silyl
 ethers studied by in situ NMR
;
_journal_issue                   14
_journal_name_full               'RSC Advances'
_journal_page_first              5941
_journal_paper_doi               10.1039/c2ra20860a
_journal_volume                  2
_journal_year                    2012
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C17 H20 N O, C7 H5 O2'
_chemical_formula_sum            'C24 H25 N O3'
_chemical_formula_weight         375.45
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 107.906(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.9196(3)
_cell_length_b                   19.4951(9)
_cell_length_c                   9.1303(5)
_cell_measurement_reflns_used    3543
_cell_measurement_temperature    123
_cell_measurement_theta_max      66.4670
_cell_measurement_theta_min      5.0794
_cell_volume                     1002.63(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
1 omega 10.00 63.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -11.6137 45.0000 30.0000 0.0000 0.0000 53

2 omega -58.00 -13.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 11.6137 -45.0000 0.0000 0.0000 0.0000 45

3 omega 14.00 61.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -11.6137 45.0000 90.0000 0.0000 0.0000 47

4 omega -123.00 -70.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -90.0000 128.0000 38.0000 0.0000 0.0000 53

5 omega -118.00 -65.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -90.0000 45.0000 120.0000 0.0000 0.0000 53

6 omega -148.00 -122.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -90.0000 -142.0000 153.0000 0.0000 0.0000 26

7 omega -165.00 -112.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -90.0000 -45.0000 0.0000 0.0000 0.0000 53

8 omega 66.00 119.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 45.0000 240.0000 0.0000 0.0000 53

9 omega 80.00 133.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -92.0000 296.0000 0.0000 0.0000 53

10 omega 124.00 168.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 45.0000 210.0000 0.0000 0.0000 44

11 omega 21.00 71.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -45.0000 300.0000 0.0000 0.0000 50

12 omega 117.00 162.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 130.0000 306.0000 0.0000 0.0000 45

13 omega 15.00 73.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -77.0000 120.0000 0.0000 0.0000 58

14 omega 21.00 54.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -139.0000 238.0000 0.0000 0.0000 33

15 omega 117.00 167.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 45.0000 60.0000 0.0000 0.0000 50

16 omega 84.00 113.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -93.0000 133.0000 0.0000 0.0000 29

17 omega 69.00 110.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 77.0000 60.0000 0.0000 0.0000 41

18 omega 76.00 119.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -37.0000 220.0000 0.0000 0.0000 43

19 omega 70.00 96.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -63.0000 176.0000 0.0000 0.0000 26

20 omega 67.00 93.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -34.0000 257.0000 0.0000 0.0000 26

21 omega 74.00 101.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -89.0000 255.0000 0.0000 0.0000 27

22 omega 81.00 108.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -92.0000 174.0000 0.0000 0.0000 27

23 omega 19.00 45.00 1.0000 23.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 93.5000 -128.0000 321.0000 0.0000 0.0000 26

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5354
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.65
_diffrn_reflns_theta_max         66.65
_diffrn_reflns_theta_min         5.09
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(3)
_refine_ls_extinction_coef       0.0121(17)
_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   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2855
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0841P)^2^+0.1355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                2584
_reflns_number_total             2855
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2ra20860a.txt
_cod_data_source_block           h237
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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_sg_symbol_H-M      'P 21'
_cod_database_code               7238686