Selective dimerization of a trinuclear mixed-metal sandwich complex: construction of an axially chiral metal skeleton.
Yamaura, Hiroshige; Yamamoto, Koji; Murahashi, Tetsuro; Chemical communications (Cambridge, England) 57 (2021) 9120–9123; doi:10.1039/d1cc03719f

data_7128854
_publ_section_title
;
 Selective dimerization of a trinuclear mixed-metal sandwich complex:
 construction of an axially chiral metal skeleton.
;
_journal_issue                   72
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9120
_journal_page_last               9123
_journal_paper_doi               10.1039/d1cc03719f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C42 H36 O Pd Pt2, 2(B F4)'
_chemical_formula_sum            'C42 H36 B2 F8 O Pd Pt2'
_chemical_formula_weight         1226.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-06-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-05 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                104.1710(9)
_cell_angle_beta                 103.2030(9)
_cell_angle_gamma                92.3928(11)
_cell_formula_units_Z            2
_cell_length_a                   10.2863(3)
_cell_length_b                   10.8987(4)
_cell_length_c                   17.5682(5)
_cell_measurement_reflns_used    52722
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.14
_cell_volume                     1849.14(10)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR97  (Burla et al.,  2007)'
_diffrn_ambient_temperature      153.15
_diffrn_detector                 CCD
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_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  0.0947
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35926
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.140
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.104
_exptl_absorpt_correction_T_max  0.380
_exptl_absorpt_correction_T_min  0.024
_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    2.204
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.178
_refine_diff_density_min         -2.761
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         6957
_refine_ls_number_restraints     358
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0501
_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^)+106.4109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6296
_reflns_number_total             6957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03719f2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7128853--7128856.cif.'
_cod_original_cell_volume        1849.13(10)
_cod_database_code               7128854
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.443
_shelx_estimated_absorpt_t_min   0.294
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C15 \\sim C16 \\sim Pt1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C27 \\sim C28 \\sim C23 \\sim C24 \\sim C25 \\sim C26: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(Pt1) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 C37, C38, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C16, Pt1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, C28, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 O1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C18(H18), C19(H19), C20(H20),
  C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92463
_shelx_fab_checksum              57752
_olex2_submission_special_instructions 'No special instructions were received'