Crystal structure of (1S)-N-(chloromethyl)-1-((4S,6aR,8aS, 8bR,9aR)-4-methoxy-6a,8a-dimethyl-1,3,4, 5,6,6a,6b,7,8,8a,9a,10,10a,10b-tetradecahydro-8bH-naphtho[2′,1′:4,5] indeno[1,2-b]oxiren-8b-yl)-N-methylethan-1-amine, C24H46ClNO5
Ning, Xue-Jing; Yang, Xiao-Bin; Du, Jiang; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1493–1494; doi:10.1515/ncrs-2020-0367

data_8105503
_publ_section_title
;
 Crystal structure of (1S)-N-(chloromethyl)-1-((4S,6aR,8aS,
 8bR,9aR)-4-methoxy-6a,8a-dimethyl-1,3,4,
 5,6,6a,6b,7,8,8a,9a,10,10a,10b-tetradecahydro-8bH-naphtho[2&#x2032;,1&#x2032;:4,5]
 indeno[1,2-b]oxiren-8b-yl)-N-methylethan-1-amine, C24H46ClNO5
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1493
_journal_page_last               1494
_journal_paper_doi               10.1515/ncrs-2020-0367
_journal_volume                  235
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'Cl, C24 H40 N O2, 3(H2 O)'
_chemical_formula_sum            'C24 H46 Cl N O5'
_chemical_formula_weight         464.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5992(3)
_cell_length_b                   9.6634(5)
_cell_length_c                   34.7499(18)
_cell_measurement_reflns_used    2264
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.187
_cell_measurement_theta_min      2.844
_cell_volume                     2551.8(2)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            16563
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_min         2.187
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 (Bruker,2016/2) was used for absorption 
correction. wR2(int) was 0.0929 before and 0.0491 after 
correction. The Ratio of minimum to maximum transmission 
is 0.7847. The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 1297 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0638P)^2^+1.2099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                3926
_reflns_number_total             5154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0367_suppl.cif
_cod_data_source_block           hs6_0m
_cod_database_code               8105503
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
;
1. 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,H) groups
2.a Free rotating group:
 O3(H3A,H3B), O4(H4C,H4D), O2(H2C,H2D)
2.b Ternary CH refined with riding coordinates:
 N1(H1), C14(H14), C8(H8), C9(H9), C16(H16), C20(H20), C3(H3)
2.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C15(H15A,H15B), C12(H12A,H12B), C7(H7A,H7B), C11(H11A,H11B),
 C1(H1A,H1B), C2(H2A,H2B)
2.d Aromatic/amide H refined with riding coordinates:
 C6(H6)
2.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;