Crystal structure of (E)-N-((2S,3S,4R,10R,13S, 17S)-17-(1-(dimethylamino) ethyl)-2,4-dihydroxy-10,13-dimethylhexadecahydro-1H-cyclopenta[a]phenanthren-3-yl)-2-methylbut-2-enamide, C24H48N2O3
Wu, Qi-Yun; Wu, Ji-Chun; Huo, Shao-Jie; He, Xi-Chen; Du, Jiang; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 513–516; doi:10.1515/ncrs-2018-0511

data_8105764
_publ_section_title
;
 Crystal structure of (E)-N-((2S,3S,4R,10R,13S, 17S)-17-(1-(dimethylamino)
 ethyl)-2,4-dihydroxy-10,13-dimethylhexadecahydro-1H-cyclopenta[a]phenanthren-3-yl)-2-methylbut-2-enamide,
 C24H48N2O3
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              513
_journal_page_last               516
_journal_paper_doi               10.1515/ncrs-2018-0511
_journal_volume                  234
_journal_year                    2019
_chemical_absolute_configuration .
_chemical_formula_moiety         'C28 H48 N2 O3'
_chemical_formula_sum            'C28 H48 N2 O3'
_chemical_formula_weight         460.68
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 98.935(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.805(3)
_cell_length_b                   10.0557(18)
_cell_length_c                   18.061(3)
_cell_measurement_reflns_used    2354
_cell_measurement_temperature    173
_cell_measurement_theta_max      19.659
_cell_measurement_theta_min      2.283
_cell_volume                     2656.2(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22053
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.314
_diffrn_reflns_theta_min         1.658
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) 
was 0.0733 before and 0.0559 after correction. The Ratio of minimum to 
maximum transmission is 0.8885. The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -2.2(17)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         10586
_refine_ls_number_restraints     645
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1011P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                6703
_reflns_number_total             10586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0511_suppl.cif
_cod_data_source_block           mo
_cod_original_cell_volume        2656.3(8)
_cod_database_code               8105764
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 3.2(17)
 -2.2(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 H28B-H27B
 2.3 with sigma of 0.02
 C27-C26 \\sim C56-C55
 with sigma of 0.02
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C27
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C26 \\sim C27: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C56) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C27) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C26) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
6.a Ternary CH refined with riding coordinates:
 C36(H36), C42(H42), C9(H9), C37(H37), C45(H45), C4(H4A), C31(H31), C8(H8),
 C30(H30), C20(H20), C32(H32), C33(H33), C14(H14), C17(H17), C48(H48), C5(H5A),
 C3(H3A), C2(H2A)
6.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C40(H40A,H40B), C11(H11A,H11B), C57(H57A,H57B), C43(H43A,
 H43B), C35(H35A,H35B), C12(H12A,H12B), C44(H44A,H44B), C1(H1B,H1C), C6(H6A,
 H6B), C34(H34A,H34B), C16(H16A,H16B), C15(H15A,H15B), C7(H7A,H7B)
6.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N1(H1A), C55(H55), C26(H26)
6.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C19(H19A,H19B,H19C), C47(H47A,H47B,H47C), C18(H18A,H18B,
 H18C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C50(H50A,H50B,H50C), C49(H49A,
 H49B,H49C), C22(H22A,H22B,H22C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C),
 C56(H56A,H56B,H56C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
6.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O4(H4), O1(H1), O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
;
;