Bridging coordination of acenaphthylene to a Pd<sub>3</sub> chain or a Pd<sub>4</sub> sheet cluster.
Yamamoto, Koji; Sugawa, Tsuyoshi; Kondo, Mio; Masaoka, Shigeyuki; Murahashi, Tetsuro; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1901–1906; doi:10.1039/d1dt04071e

data_7709295
_publ_section_title
;
 Bridging coordination of acenaphthylene to a Pd<sub>3</sub> chain or a
 Pd<sub>4</sub> sheet cluster.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1901
_journal_page_last               1906
_journal_paper_doi               10.1039/d1dt04071e
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C101 H55 B2 F48 N2 Pd3'
_chemical_formula_sum            'C101 H55 B2 F48 N2 Pd3'
_chemical_formula_weight         2549.30
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-07-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2021-10-19 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.9552(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.5164(6)
_cell_length_b                   27.9490(10)
_cell_length_c                   24.4264(10)
_cell_measurement_reflns_used    65595
_cell_measurement_temperature    129
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.00
_cell_volume                     9658.0(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_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 Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      129
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            134093
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         3.002
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.432
_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    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5020.00
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.23
_refine_diff_density_min         -2.20
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1371
_refine_ls_number_reflns         21915
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1030P)^2^+32.9668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1944
_refine_ls_wR_factor_ref         0.2171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15410
_reflns_number_total             21915
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1dt04071e2.cif
_cod_data_source_block           R378
_cod_depositor_comments
'Adding full bibliography for 7709295--7709296.cif.'
_cod_database_code               7709295
_olex2_refinement_description
;
1. Restrained distances
 C93-C94 = C94-C95 = C95-C96 = C96-C97 = C97-C98 = C98-C93
 1.39 with sigma of 0.02
 C99-C100 = C100-C101
 1.39 with sigma of 0.02
 C93-C95
 2.1665 with sigma of 0.04
 C94-C96
 2.4244 with sigma of 0.04
 C95-C97
 2.3201 with sigma of 0.04
 C96-C98
 2.2461 with sigma of 0.04
 C97-C93
 2.5478 with sigma of 0.04
 C98-C94
 2.3943 with sigma of 0.04
 C99-C101
 2.424 with sigma of 0.04
2. Restrained planarity
 C93, C94, C95, C96, C97, C98
 with sigma of 0.02
3. Rigid bond restraints
 C93, C94, C95, C96, C97, C98
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C99, C100, C101
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C99 \\sim C100 \\sim C101: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C99) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: F2A(0.5) F2B(0.5) F1A(0.5) F1B(0.5) F3B(0.5) F3A(0.5) F28B(0.5)
 F26A(0.5) F27A(0.5) F26B(0.5) F25A(0.5) F25B(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C30(H30),
  C32(H32), C34(H34), C38(H38), C40(H40), C42(H42), C46(H46), C48(H48),
 C50(H50), C54(H54), C56(H56), C58(H58), C62(H62), C64(H64), C66(H66), C70(H70),
  C72(H72), C74(H74), C78(H78), C80(H80), C82(H82), C86(H86), C88(H88),
 C90(H90), C93(H93), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98), C99(H99),
  C100(H100), C101(H101)
6.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              58948
_shelx_hkl_checksum              19716
_olex2_submission_special_instructions 'No special instructions were received'