A rapid pathway to molecular complexity: a palladium-catalyzed six-fold domino process to access polycyclic frameworks.
Goel, Komal; Satyanarayana, Gedu; Chemical communications (Cambridge, England) 61 (2025) 536–539; doi:10.1039/d4cc05380j

data_7134029
_publ_section_title
;
 A rapid pathway to molecular complexity: a palladium-catalyzed six-fold
 domino process to access polycyclic frameworks.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              536
_journal_page_last               539
_journal_paper_doi               10.1039/d4cc05380j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C46 H34 O4'
_chemical_formula_sum            'C46 H34 O4'
_chemical_formula_weight         650.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-18
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-04 deposited with the CCDC.	2024-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.896(3)
_cell_length_b                   12.2890(10)
_cell_length_c                   16.7731(15)
_cell_measurement_reflns_used    5618
_cell_measurement_temperature    298
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      2.38
_cell_volume                     6986.8(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-IV Photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.140
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1024 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.8944.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0639P)^2^+4.4156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3525
_reflns_number_total             6153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05380j2.cif
_cod_data_source_block           mo_gs_kg_390_b1_0m
_cod_depositor_comments          'Adding full bibliography for 7134029.cif.'
_cod_database_code               7134029
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.976
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-O4A \\sim C42-O4
 with sigma of 0.02
 C46A-O4A \\sim C46-O4
 with sigma of 0.02
 C42-C46A \\sim C42-C46
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C46A \\sim O4A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C46 \\sim O4: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(C46A) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Uanis(C46) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
4. Others
 Sof(C46)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(O4)=1-FVAR(1)
 Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(O4A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C11(H11), C28(H28), C22(H22), C29(H29), C8(H8), C10(H10), C19(H19),
 C20(H20), C9(H9), C5(H5), C36(H36), C7(H7), C39(H39), C37(H37), C45(H45),
 C3(H3), C4(H4), C38(H38), C41(H41), C44(H44), C43(H43)
5.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C23(H23A,H23B,H23C), C46A(H46A,H46B,H46C), C1(H1A,H1B,
 H1C), C46(H46D,H46E,H46F)
;
_shelx_res_checksum              2729
_shelx_hkl_checksum              4582
_olex2_exptl_crystal_mounting_method 'Nylon loop used'
_olex2_submission_special_instructions 'No special instructions were received'