Electronic versus steric control in palladium complexes of carboranyl phosphine-iminophosphorane ligands.
Rodríguez-Rey, José Luis; Esteban-Gómez, David; Platas-Iglesias, Carlos; Sousa-Pedrares, Antonio; Dalton transactions (Cambridge, England : 2003) 48 (2019) 486–503; doi:10.1039/c8dt04006k

data_7048286
_publ_section_title
;
 Electronic versus steric control in palladium complexes of carboranyl
 phosphine-iminophosphorane ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              486
_journal_page_last               503
_journal_paper_doi               10.1039/c8dt04006k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C27.5 H34 B10 Cl3 N P2 Pd'
_chemical_formula_weight         761.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-07-12 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5388(16)
_cell_length_b                   15.5576(14)
_cell_length_c                   26.972(2)
_cell_measurement_reflns_used    1988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.46
_cell_volume                     6940.0(11)
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_collection       'BRUKER APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT-2014
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1230
_diffrn_reflns_av_unetI/netI     0.0876
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            47928
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.688
_diffrn_reflns_theta_min         1.510
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.8250
_exptl_absorpt_correction_T_min  0.6693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Sheldrick, G.M. SADABS: Program for absorption correction
 using area detector data. University of G\"ottingen, Germany, 1996.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.698
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         6592
_refine_ls_number_restraints     668
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0001P)^2^+36.1719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4388
_reflns_number_total             6592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04006k2.cif
_cod_data_source_block           Pd4
_cod_depositor_comments
'Adding full bibliography for 7048284--7048289.cif.'
_cod_original_formula_sum        'C27.50 H34 B10 Cl3 N P2 Pd'
_cod_database_code               7048286
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.611
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              91610