Di- and trinuclear sandwich complexes of a cross-conjugated fulvene.
Kudo, Eiji; Oba, Yuki; Yamamoto, Koji; Murahashi, Tetsuro; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1568–1573; doi:10.1039/d2dt03521a

data_7712150
_publ_section_title
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 Di- and trinuclear sandwich complexes of a cross-conjugated fulvene.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1568
_journal_page_last               1573
_journal_paper_doi               10.1039/d2dt03521a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C22 H29 N3 Pd3, 2(B F4), C7 H8'
_chemical_formula_sum            'C29 H37 B2 F8 N3 Pd3'
_chemical_formula_weight         920.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-07
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2022-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.6707(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7178(7)
_cell_length_b                   11.1501(5)
_cell_length_c                   18.1341(8)
_cell_measurement_reflns_used    24046
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.63
_cell_volume                     3305.7(2)
_computing_cell_refinement       'RAPID AUTO (Rigaku, ????)'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO (Rigaku, ????)'
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.628
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.476
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3785
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0507
_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^)+(0.1111P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2960
_reflns_number_total             3785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03521a2.cif
_cod_data_source_block           shelxl_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7712149--7712153.cif.'
_cod_database_code               7712150
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.713
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H10A,H10B,H10C} of C10, {H7A,H7B,H7C} of C7, {H12A,H12B,
  H12C} of C12, {H8A,H8B,H8C} of C8
 At 1.5 times of:
  {H13A,H13B,H13C} of C13
2. Restrained distances
 C13-C14
 1.51 with sigma of 0.02
 C14-C15 = C14-C19 = C16-C17
 1.39 with sigma of 0.02
 C15-C16 = C17-C18 = C18-C19
 1.38 with sigma of 0.02
 C13-C15 = C13-C19
 2.52 with sigma of 0.04
 C14-C16
 2.42 with sigma of 0.04
 C14-C18
 2.41 with sigma of 0.04
 C15-C17
 2.39 with sigma of 0.04
 C16-C18 = C17-C19
 2.4 with sigma of 0.04
 C14-C15 \\sim C15-C16 \\sim C16-C17 \\sim C17-C18 \\sim C18-C19 \\sim C19-C14
 with sigma of 0.02
 C14-C18 \\sim C14-C16 \\sim C19-C17 \\sim C15-C19 \\sim C16-C18 \\sim C15-C17
 with sigma of 0.04
 C13-C19 \\sim C13-C15
 with sigma of 0.04
3. Restrained planarity
 C13, C14, C15, C16, C17, C18, C19
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C13, C14, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H12C(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 H13C(0.5) C14(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5)
 C18(0.5) H18(0.5) C19(0.5) H19(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19)
7.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              60282
_olex2_submission_special_instructions 'No special instructions were received'