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_7712149
_publ_section_title
;
 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         'C40 H34 N2 Pd2, 4(B0.5 F2), 2(C H3 N O2)'
_chemical_formula_sum            'C42 H40 B2 F8 N4 O4 Pd2'
_chemical_formula_weight         1051.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-11-28
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.0364(17)
_cell_length_b                   14.3700(9)
_cell_length_c                   19.3410(12)
_cell_measurement_reflns_used    35516
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      3.20
_cell_volume                     8626.0(9)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.15
_diffrn_detector                 'Rigaku IP'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            RAPID
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1636
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            119367
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.095
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR(Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       block
_exptl_crystal_F_000             4208
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.277
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.00083(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         9874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0743
_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^)+(0.1240P)^2^+5.2924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4815
_reflns_number_total             9874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03521a2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7712149--7712153.cif.'
_cod_database_code               7712149
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.824
_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.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C20(H20), C30(H30), C29(H29), C28(H28), C27(H27),
 C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C2(H2), C1(H1),
 C4(H4), C3(H3), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C19(H19)
2.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C)
;
_shelx_res_checksum              27291
_olex2_submission_special_instructions 'No special instructions were received'