Oxidation of cholesterol and O-protected derivatives by the environmental pollutant NO2˙.
Zalewski, A. N.; Nathanael, J. G.; White, J. M.; Wille, U.; Chemical communications (Cambridge, England) 52 (2016) 4060–4063; doi:10.1039/c5cc09663d

data_7118766
_publ_section_title
;
 Oxidation of cholesterol and O-protected derivatives by the environmental
 pollutant NO2&#x02D9;.
;
_journal_issue                   21
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4060
_journal_page_last               4063
_journal_paper_doi               10.1039/c5cc09663d
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration rm
_chemical_formula_sum            'C28 H47 N3 O6'
_chemical_formula_weight         521.68
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-13 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.223(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5615(3)
_cell_length_b                   10.1140(3)
_cell_length_c                   12.3397(3)
_cell_measurement_reflns_used    5865
_cell_measurement_temperature    130.0(1)
_cell_measurement_theta_max      34.0680
_cell_measurement_theta_min      3.3750
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19248
_diffrn_reflns_point_group_measured_fraction_full 0.754
_diffrn_reflns_point_group_measured_fraction_max 0.636
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.636
_diffrn_reflns_theta_min         3.338
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.4955
_exptl_crystal_size_mid          0.4323
_exptl_crystal_size_min          0.2067
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1531 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.4(6)
_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     340
_refine_ls_number_reflns         8954
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.2292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.297
_reflns_Friedel_fraction_full    0.480
_reflns_Friedel_fraction_max     0.305
_reflns_number_gt                7373
_reflns_number_total             8954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc09663d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7118766.cif.'
_cod_database_code               7118766
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'Anton Zalewski (UW) AZ-49A-01'
_shelx_res_checksum              61784