Understanding the Solution and Solid-State Structures of Pd and Pt PSiP Pincer-Supported Hydrides.
Suh, Hee-Won; Balcells, David; Edwards, Alison J.; Guard, Louise M.; Hazari, Nilay; Mader, Elizabeth A.; Mercado, Brandon Q.; Repisky, Michal; Inorganic chemistry 54 (2015) 11411–11422; doi:10.1021/acs.inorgchem.5b02073

data_4344450
_publ_contact_author
;
 Prof. Nilay Hazari         
 The Department of Chemistry 
 Yale University 
 P. O. Box 208107 
 New Haven 
 Connecticut 06520 USA.
;
_publ_section_title
;
 Understanding the Solution and Solid-State Structures of Pd and Pt PSiP
 Pincer-Supported Hydrides.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11411
_journal_page_last               11422
_journal_paper_doi               10.1021/acs.inorgchem.5b02073
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C25 H40 P2 Pd Si'
_chemical_formula_sum            'C25 H40 P2 Pd Si'
_chemical_formula_weight         537.00
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.714(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3892(13)
_cell_length_b                   9.00120(10)
_cell_length_c                   14.9432(2)
_cell_measurement_reflns_used    104965
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2599.16(18)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics
;
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program
(2009). J. Appl. Cryst., 42, 339-341.
;
_computing_publication_material  'SHELXL-2013/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            120045
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.012
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.310
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0142P)^2^+3.5577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5745
_reflns_number_total             5971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02073_si_002.cif
_cod_data_source_block           '_(iPrPSiP)PdH'
_cod_depositor_comments
'Adding full bibliography for 4344446--4344451.cif.'
_cod_database_code               4344450
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.717
_shelx_estimated_absorpt_t_max   0.769
_shelx_res_checksum              16031
_shelx_hkl_checksum              38805