Synthesis of the ABC ring system of kadlongilactones.
Li, Liang; Li, Pengfei; Li, Tianhao; Zhang, Mingxiao; Liu, Wenjie; Li, Jing; Wang, Liang; Chen, Yue; Organic & biomolecular chemistry 21 (2023) 1704–1708; doi:10.1039/d2ob01701f

data_7159133
_publ_section_title
;
 Synthesis of the ABC ring system of kadlongilactones.
;
_journal_issue                   8
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1704
_journal_page_last               1708
_journal_paper_doi               10.1039/d2ob01701f
_journal_volume                  21
_journal_year                    2023
_chemical_formula_moiety         'C17 H24 O3'
_chemical_formula_sum            'C17 H24 O3'
_chemical_formula_weight         276.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-30 deposited with the CCDC.	2023-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.749(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9019(2)
_cell_length_b                   7.00790(10)
_cell_length_c                   17.7102(3)
_cell_measurement_reflns_used    3699
_cell_measurement_temperature    102(5)
_cell_measurement_theta_max      75.2390
_cell_measurement_theta_min      5.1150
_cell_volume                     1440.74(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      102(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -35.00  33.00   0.50    2.00    --    0.00 -82.00   0.00  136
  2  \w    -35.00  38.00   0.50    2.00    --    0.00  82.00 -60.00  146
  3  \w     26.00 115.00   0.50    7.00    --  101.90 -38.00-180.00  178
  4  \w     64.00 131.00   0.50    7.00    --  101.90 -82.00  30.00  134
  5  \w     18.00  58.00   0.50    7.00    --  101.90 -82.00  30.00   80
  6  \w     15.00 121.00   0.50    7.00    --  101.90 -57.00  30.00  212
  7  \w     12.00 135.00   0.50    7.00    --  101.90 -19.00-120.00  246
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1143150000
_diffrn_orient_matrix_UB_12      0.0004881000
_diffrn_orient_matrix_UB_13      0.0274022000
_diffrn_orient_matrix_UB_21      -0.0668817000
_diffrn_orient_matrix_UB_22      -0.0340565000
_diffrn_orient_matrix_UB_23      -0.0837790000
_diffrn_orient_matrix_UB_31      0.0102936000
_diffrn_orient_matrix_UB_32      -0.2170833000
_diffrn_orient_matrix_UB_33      0.0131622000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5017
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        66.997
_diffrn_reflns_theta_max         66.997
_diffrn_reflns_theta_min         3.808
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.306
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.306
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0727
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2129
_reflns_number_total             2455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob01701f2.cif
_cod_data_source_block           ll-7-8-1
_cod_depositor_comments
;
Adding full bibliography for 7159130--7159137.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C68 H96 O12'
_cod_original_formula_weight         1105.44
_cod_original_formula_moiety         '4(C17 H24 O3)'
_cod_original_formula_units_Z            1
_cod_database_code               7159133
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 94.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C004(H004), C005(H005), C00B(H00N), C00C(H00C)
2.b Secondary CH2 refined with riding coordinates:
 C008(H00I,H00K), C00A(H00L,H00M), C00D(H00O,H00P), C00F(H00D,H00E), C00K(H00A,
 H00B)
2.c Aromatic/amide H refined with riding coordinates:
 C00J(H00J)
2.d Idealised Me refined as rotating group:
 C007(H00F,H00G,H00H), C00G(H00Q,H00R,H00S), C00H(H00T,H00U,H00V)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.027
_oxdiff_exptl_absorpt_empirical_full_min 0.320