P-stereocontrolled synthesis of oligo(nucleoside N3′\ρightarrow O5′ phosphoramidothioate)s ‒ opportunities and limitations
Radzikowska, Ewa; Kaczmarek, Renata; Korczyński, Dariusz; Krakowiak, Agnieszka; Mikołajczyk, Barbara; Baraniak, Janina; Guga, Piotr; Wheeler, Kraig A.; Pawlak, Tomasz; Nawrot, Barbara; RSC Advances 10 (2020) 35185–35197; doi:10.1039/D0RA04987E

data_7241297
_publ_section_title
;
 P-stereocontrolled synthesis of oligo(nucleoside N3&#x2032;\\rightarrow
 O5&#x2032; phosphoramidothioate)s -- opportunities and limitations
;
_journal_issue                   58
_journal_name_full               'RSC Advances'
_journal_page_first              35185
_journal_page_last               35197
_journal_paper_doi               10.1039/D0RA04987E
_journal_volume                  10
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H55 N8 O13 P S, 2(C H4 O)'
_chemical_formula_sum            'C50 H63 N8 O15 P S'
_chemical_formula_weight         1079.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-09 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.346(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2758(6)
_cell_length_b                   14.8286(8)
_cell_length_c                   18.2612(10)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.43
_cell_measurement_theta_min      2.45
_cell_volume                     2745.6(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2018.7-2 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2017)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'XSEED (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'Bruker Photon II CPAD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CPAD Area Detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57523
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.425
_diffrn_reflns_theta_min         2.452
_diffrn_source                   'Microsource IuS Incoatec 3.0'
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       needle
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.031
_exptl_transmission_factor_max   0.7410
_exptl_transmission_factor_min   0.5867
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 4079 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.176(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.802
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         10009
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.797
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.1196
_refine_ls_shift/su_max          0.142
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3665
_refine_ls_wR_factor_ref         0.3702
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                9499
_reflns_number_total             10009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04987e2.cif
_cod_data_source_block           19demb02
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7241297
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              66185