Synthesis and characterization of <i>closo</i>-decahydrido-decaborate-phosphine mediated by palladium(0) complexes.
Haidar Ahmad, Zainab; Cordier, Marie; Naoufal, Daoud; Darcel, Christophe; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12135–12140; doi:10.1039/d5dt01302j

data_7719107
_publ_section_title
;
 Synthesis and characterization of
 <i>closo</i>-decahydrido-decaborate-phosphine mediated by palladium(0)
 complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12135
_journal_page_last               12140
_journal_paper_doi               10.1039/d5dt01302j
_journal_volume                  54
_journal_year                    2025
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H24 B10 P, C16 H36 N'
_chemical_formula_sum            'C34 H60 B10 N P'
_chemical_formula_weight         621.90
_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   mixed
_atom_sites_solution_primary     dual
_audit_update_record
;
2025-06-04 deposited with the CCDC.	2025-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.104(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5958(14)
_cell_length_b                   14.1604(10)
_cell_length_c                   17.7746(15)
_cell_measurement_reflns_used    8838
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5024
_cell_measurement_theta_min      2.4262
_cell_measurement_wavelength     0.710730
_cell_volume                     3838.1(5)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2023)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      0.0622146
_diffrn_orient_matrix_UB_12      0.0063163
_diffrn_orient_matrix_UB_13      0.0286087
_diffrn_orient_matrix_UB_21      -0.0204249
_diffrn_orient_matrix_UB_22      0.0318015
_diffrn_orient_matrix_UB_23      0.0433268
_diffrn_orient_matrix_UB_31      -0.0040898
_diffrn_orient_matrix_UB_32      -0.0627355
_diffrn_orient_matrix_UB_33      0.0248433
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35703
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.344
_diffrn_source_current           1.00
_diffrn_source_power             50.0
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         7272
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+3.7778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                5500
_reflns_number_total             7272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5dt01302j2.cif
_cod_data_source_block           ZH103
_cod_depositor_comments
'Adding full bibliography for 7719107--7719112.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7719107
_shelx_res_checksum              48361
_shelx_hkl_checksum              12528