A highly constrained cis-dihydride platinum complex trapped by cooperative gold/platinum dihydrogen activation
Hidalgo, Nereida; de la Cruz-Martinez, Felipe; Martín, M. Trinidad; Nicasio, M. Carmen; Campos, Jesús; Chemical Communications  (2022) –; doi:10.1039/D2CC03089F

data_7130368
_publ_section_title
;
 A highly constrained cis-dihydride platinum complex trapped by
 cooperative gold/platinum dihydrogen activation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03089F
_journal_year                    2022
_chemical_formula_sum            'C136.5 H172 Au F6 N O4 P3 Pt S2'
_chemical_formula_weight         2553.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-07-14 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.909(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9936(7)
_cell_length_b                   44.882(2)
_cell_length_c                   21.8761(12)
_cell_measurement_reflns_used    9542
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.27
_cell_volume                     13392.3(12)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            141684
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.824
_diffrn_source                   'IuS 3.0 Microfocus Source'
_exptl_absorpt_coefficient_mu    2.262
_exptl_absorpt_correction_T_max  0.4912
_exptl_absorpt_correction_T_min  0.3591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' Apex3 v2016.9-0 (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       needle
_exptl_crystal_F_000             5272
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The unit cell contains 22 toluene molecules which have
been treated as a diffuse contribution to the overall scattering
without specific atom positions by SQUEEZE/PLATON. These
molecules are found in a volume of 4802 A3 in two voids
per unit cell. This information has been included in the
moiety and sum forumla'
;
_refine_diff_density_max         4.046
_refine_diff_density_min         -2.935
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       0.0105(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.558
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         24233
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.564
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0967
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1334P)^2^+37.0010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2911
_refine_ls_wR_factor_ref         0.2950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21686
_reflns_number_total             24233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03089f2.cif
_cod_data_source_block           jcm12121a_v2_sq
_cod_original_cell_volume        13392.2(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C136.50 H172 Au F6 N O4 P3 Pt S2'
_cod_database_code               7130368
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              87599
_shelx_hkl_checksum              13924
_shelx_fab_checksum              98173