Cationic dinuclear complexes [M<sub>2</sub>(PCP)<sub>2</sub><i>μ</i>-Cl][GaCl<sub>4</sub>] of the group 10 elements. metallophilic interactions and catalytic dehydrogenation of Me<sub>2</sub>NHBH<sub>3</sub>.
Meyer, Fabio; Puylaert, Pim; Duvinage, Daniel; Hupf, Emanuel; Beckmann, Jens; Chemical communications (Cambridge, England) 60 (2024) 12912–12915; doi:10.1039/d4cc04296d

data_7133843
_publ_section_title
;
 Cationic dinuclear complexes
 [M<sub>2</sub>(PCP)<sub>2</sub><i>&#x3bc;</i>-Cl][GaCl<sub>4</sub>] of
 the group 10 elements. metallophilic interactions and catalytic
 dehydrogenation of Me<sub>2</sub>NHBH<sub>3</sub>.
;
_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12912
_journal_page_last               12915
_journal_paper_doi               10.1039/d4cc04296d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C60 H46 Cl P4 Pd2, 2(Cl2 Ga0.5)'
_chemical_formula_sum            'C60 H46 Cl5 Ga P4 Pd2'
_chemical_formula_weight         1350.62
_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   geom
_audit_creation_date             2022-12-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-09-15 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                77.139(2)
_cell_angle_beta                 61.775(2)
_cell_angle_gamma                89.651(2)
_cell_formula_units_Z            2
_cell_length_a                   15.1433(6)
_cell_length_b                   15.3082(5)
_cell_length_c                   15.6366(6)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.21
_cell_volume                     3092.9(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 V2019.1-01 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Venture D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            71038
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.059
_diffrn_reflns_theta_max         25.059
_diffrn_reflns_theta_min         2.639
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0784 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.8876.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.570
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         10960
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0492P)^2^+32.0287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9678
_reflns_number_total             10960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04296d2.cif
_cod_data_source_block           meyerf221212_0m
_cod_depositor_comments
'Adding full bibliography for 7133840--7133844.cif.'
_cod_database_code               7133843
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.763
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C73A)
\\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl7A) \\sim Ueq, Uanis(Ga3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H72(0.5) H72A(0.5) C73(0.5) H73(0.5) C73A(0.5) H73A(0.5) C74(0.5)
 H74(0.5) C74A(0.5) H74A(0.5) C75(0.5) H75(0.5) C75A(0.5) H75A(0.5) Ga1(0.25)
 Ga2(0.25) Cl1(0.5) Cl2(0.5) Cl3(0.5) Cl4(0.5) Ga3(0.15) Ga4(0.35) Cl5(0.35)
 Cl5A(0.15) Cl6(0.5) Cl7(0.35) Cl7A(0.15) Cl8(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C21(H21), C22(H22), C23(H23), C24(H24),
 C25(H25), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42),
  C43(H43), C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C62(H62), C63(H63), C64(H64), C71(H71), C72(H72), C72(H72A),
 C73(H73), C73A(H73A), C74(H74), C74A(H74A), C75(H75), C75A(H75A), C81(H81),
 C82(H82), C83(H83), C84(H84), C85(H85), C91(H91), C92(H92), C93(H93), C94(H94),
  C95(H95), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19478
_shelx_hkl_checksum              60286
_shelx_fab_checksum              55154
_olex2_submission_special_instructions 'No special instructions were received'