Crystal structure of (4S,4aS,6aR,6bR,12aS,12bR,14aS,14bR)-3,3,6a,6b,9,9,12a-heptamethyloctadecahydro-1H,3H-4,14b-ethanophenanthro[1,2-h]isochromene-1(6bH)-one, C30H48O2
He, Kang; Fan, Lin-Lin; Wu, Tian-Tai; Zhang, Qi-Long; Zou, Juan; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1005–1007; doi:10.1515/ncrs-2019-0217

data_8105919
_publ_section_title
;
 Crystal structure of
 (4S,4aS,6aR,6bR,12aS,12bR,14aS,14bR)-3,3,6a,6b,9,9,12a-heptamethyloctadecahydro-1H,3H-4,14b-ethanophenanthro[1,2-h]isochromene-1(6bH)-one,
 C30H48O2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1005
_journal_page_last               1007
_journal_paper_doi               10.1515/ncrs-2019-0217
_journal_volume                  234
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H48 O2'
_chemical_formula_sum            'C30 H48 O2'
_chemical_formula_weight         440.68
_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   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.8192(12)
_cell_length_b                   16.4915(17)
_cell_length_c                   28.832(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.25
_cell_volume                     5144.3(9)
_computing_cell_refinement       'SAINT (Brucker, 2012)[1]'
_computing_data_collection       'APEX2 (Brucker, 2012)[1]'
_computing_data_reduction        'SAINT (Brucker, 2012)[1]'
_computing_molecular_graphics    'Diamond 4.0 [4]'
_computing_publication_material  'SHELXL-2014/7 [3]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0862
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            39401
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.876
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.9838
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 1861 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.2(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         9050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.5246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5738
_reflns_number_total             9050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0217_suppl.cif
_cod_data_source_block           a
_cod_depositor_comments
;

2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C60 H96 O4'
_cod_original_formula_weight         881.36
_cod_original_formula_moiety         'C30 H48 O2, C30 H48 O2'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5144.4(10)
_cod_database_code               8105919
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C5'(H5'), C9'(H9'), C9(H9), C13'(H13'), C13(H13), C17'(H17'),
 C17(H17), C20(H20), C20'(H20')
2.b Secondary CH2 refined with riding coordinates:
 C1'(H1'A,H1'B), C1(H1A,H1B), C2(H2A,H2B), C2'(H2'A,H2'B), C3'(H3'A,H3'B),
 C3(H3A,H3B), C6'(H6'A,H6'B), C6(H6A,H6B), C7'(H7'A,H7'B), C7(H7A,H7B),
 C11'(H11A,H11B), C11(H11C,H11D), C12'(H12A,H12B), C12(H12C,H12D), C15'(H15A,
 H15B), C15(H15C,H15D), C16'(H16A,H16B), C16(H16C,H16D), C19(H19C,H19D),
 C19'(H19A,H19B), C21'(H21A,H21B), C21(H21C,H21D)
2.c Me refined with riding coordinates:
 C23(H23D,H23E,H23F), C23'(H23A,H23B,H23C), C24'(H24A,H24B,H24C), C24(H24D,
 H24E,H24F), C27'(H27A,H27B,H27C), C27(H27D,H27E,H27F), C29(H29D,H29E,H29F),
 C29'(H29A,H29B,H29C), C30'(H30A,H30B,H30C), C30(H30D,H30E,H30F)
2.d Idealised Me refined as rotating group:
 C25'(H25A,H25B,H25C), C25(H25D,H25E,H25F), C26(H26D,H26E,H26F), C26'(H26A,
 H26B,H26C)
;
_shelx_res_checksum              83623
_shelx_hkl_checksum              12014
_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
;
;