A general approach to the synthesis of enantiopure 19-nor-Vitamin D3 and its C-2 phosphate analogs prepared from cyclohexadienyl sulfone
Vikas Sikervar; James C. Fleet; Philip Fuchs; Chem.Commun. 48 (2012) 9077–; doi:10.1039/c2cc33054g

data_7108253
_publ_section_title
;
 A general approach to the synthesis of enantiopure 19-nor-Vitamin D3 and
 its C-2 phosphate analogs prepared from cyclohexadienyl sulfone
;
_journal_name_full               Chem.Commun.
_journal_page_first              9077
_journal_paper_doi               10.1039/c2cc33054g
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H38 O6 S1 Si1'
_chemical_formula_sum            'C24 H38 O6 S Si'
_chemical_formula_weight         482.72
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 92.199(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3827(5)
_cell_length_b                   6.2563(3)
_cell_length_c                   16.7955(12)
_cell_measurement_reflns_used    4246
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      66
_cell_measurement_theta_min      2
_cell_volume                     1300.19(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
ORTEP (Johnson, 1976)
PLATON (Spek, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
Direct methods (SIR2004, Burla et al., 2005)
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_measured_fraction_theta_full 0.9660
_diffrn_measured_fraction_theta_max 0.9660
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter
chi circle and a 200 degree curved image plate at a fixed
distance of 127.4mm. Strategy was optimized using the
CrystalClear software. The completeness is the best
that can be obtained with this geometry. The missing data are not cusp
data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number
of observed data as inconsistent equivalents are removed
from the data set and not included in the collected total
;
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13412
_diffrn_reflns_theta_full        60.0
_diffrn_reflns_theta_max         66.58
_diffrn_reflns_theta_min         2.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  0.9644
_exptl_absorpt_correction_T_min  0.6903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.37
_refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_d_res_high            0.89
_refine_ls_extinction_coef       0.50E-03
_refine_ls_extinction_method     'SHELXL97 (Sheldrick 2008)'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3639
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.073
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+1.3724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.173
_refine_ls_wR_factor_ref         0.178
_reflns_Friedel_coverage         1.0000
_reflns_number_gt                3362
_reflns_number_total             3639
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            c2cc33054g.txt
_cod_data_source_block           BOC
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_formula_sum        'C24 H38 O6 S1 Si1'
_cod_database_code               7108253