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_7133842
_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 Pt2, Cl4 Ga'
_chemical_formula_sum            'C60 H46 Cl5 Ga P4 Pt2'
_chemical_formula_weight         1528.00
_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             2022-12-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-09-15 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                70.1200(10)
_cell_angle_beta                 86.2630(10)
_cell_angle_gamma                89.4130(10)
_cell_formula_units_Z            2
_cell_length_a                   13.4598(4)
_cell_length_b                   15.8581(4)
_cell_length_c                   16.9458(5)
_cell_measurement_reflns_used    9653
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      33.20
_cell_measurement_theta_min      2.89
_cell_volume                     3393.97(17)
_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_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            86562
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.829
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.2801.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.860
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         13819
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+6.4061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12885
_reflns_number_total             13819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04296d2.cif
_cod_data_source_block           meyerf220425_0m
_cod_depositor_comments
'Adding full bibliography for 7133840--7133844.cif.'
_cod_database_code               7133842
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.248
_shelx_estimated_absorpt_t_min   0.196
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C40-C41A \\sim C42A-C43 \\sim C44A-C45A
 with sigma of 0.02
 C40-C41 \\sim C42-C43 \\sim C44-C45
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C83A) = Uanis(C84A) = Uanis(C85A) = Uanis(C82A) = Uanis(C81A) =
Uanis(C80A)
Uanis(C90) = Uanis(C91) = Uanis(C92) = Uanis(C93) = Uanis(C94) = Uanis(C95)
Uanis(C30) = Uanis(C35A) = Uanis(C34A) = Uanis(C34) = Uanis(C31) = Uanis(C31A)
= Uanis(C33A) = Uanis(C33) = Uanis(C32A) = Uanis(C32) = Uanis(C35)
Uanis(C90A) = Uanis(C91A) = Uanis(C92A) = Uanis(C93A) = Uanis(C94A) =
Uanis(C95A)
Uanis(C60) = Uanis(C61) = Uanis(C62) = Uanis(C63) = Uanis(C64) = Uanis(C65)
4. Rigid body (RIGU) restrains
 C72A, C73, C74A, C75A, C70, C71A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C74, C75, C70, C71, C72, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl09(0.5) C41(0.5) H41(0.5) C42(0.5) H42(0.5) H43A(0.5) H43(0.5)
 C44(0.5) H44(0.5) C45(0.5) H45(0.5) H73(0.5) H73A(0.5) C72A(0.5) H72A(0.5)
 C71A(0.5) H71A(0.5) C41A(0.5) H41A(0.5) C42A(0.5) H42A(0.5) C44A(0.5)
 H44A(0.5) C45A(0.5) H45A(0.5) C81A(0.5) H81A(0.5) C82A(0.5) H82A(0.5)
 C84A(0.5) H84A(0.5) C85A(0.5) H85A(0.5) C85(0.5) H85(0.5) C81(0.5) H81(0.5)
 C84(0.5) H84(0.5) C82(0.5) H82(0.5) C83(0.5) H83(0.5) C83A(0.5) H83A(0.5)
 C93A(0.5) H93A(0.5) C92A(0.5) H92A(0.5) C93(0.5) H93(0.5) C94A(0.5) H94A(0.5)
 C92(0.5) H92(0.5) C94(0.5) H94(0.5) C90(0.5) C90A(0.5) C95(0.5) H95(0.5)
 C91A(0.5) H91A(0.5) C91(0.5) H91(0.5) C95A(0.5) H95A(0.5) C75(0.5) H75(0.5)
 C75A(0.5) H75A(0.5) C71(0.5) H71(0.5) C74(0.5) H74(0.5) C74A(0.5) H74A(0.5)
 C72(0.5) H72(0.5) C32A(0.5) H32A(0.5) C33A(0.5) H33A(0.5) C33(0.5) H33(0.5)
 C34A(0.5) H34A(0.5) C32(0.5) H32(0.5) C35A(0.5) H35A(0.5) C34(0.5) H34(0.5)
 C31A(0.5) H31A(0.5) C35(0.5) H35(0.5) C31(0.5) H31(0.5) Cl4(0.5) Cl2(0.5)
 Cl3(0.5) Ga4(0.5) Cl5(0.5) Ga7(0.5) Cl8(0.5) Cl9(0.5) Cl11(0.5) C80(0.5)
 C80A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C101(H101), C104(H104), C13(H13), C105(H105), C63(H63), C54(H54), C14(H14),
 C12(H12), C51(H51), C25(H25), C62(H62), C64(H64), C55(H55), C102(H102),
 C103(H103), C41(H41), C42(H42), C43(H43A), C43(H43), C44(H44), C45(H45),
 C24(H24), C53(H53), C22(H22), C23(H23), C73(H73), C73(H73A), C52(H52),
 C21(H21), C72A(H72A), C71A(H71A), C41A(H41A), C42A(H42A), C44A(H44A),
 C45A(H45A), C81A(H81A), C82A(H82A), C84A(H84A), C85A(H85A), C85(H85), C81(H81),
  C84(H84), C82(H82), C83(H83), C83A(H83A), C93A(H93A), C92A(H92A), C93(H93),
 C94A(H94A), C92(H92), C94(H94), C95(H95), C91A(H91A), C91(H91), C95A(H95A),
 C75(H75), C75A(H75A), C71(H71), C74(H74), C74A(H74A), C72(H72), C32A(H32A),
 C33A(H33A), C33(H33), C34A(H34A), C32(H32), C35A(H35A), C34(H34), C31A(H31A),
 C35(H35), C31(H31)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25870
_shelx_hkl_checksum              8198
_shelx_fab_checksum              90816
_olex2_submission_special_instructions 'No special instructions were received'