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_4344451
_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         '2(C37 H56 P2 Pt1 Si)C5 H12'
_chemical_formula_sum            'C79 H124 P4 Pt2 Si2'
_chemical_formula_weight         1644.10
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     known
_atom_sites_solution_secondary   known
_audit_creation_date             2015-08-17
_audit_creation_method           'LaueG software + CRYSTALS_ver_14.61'
_cell_angle_alpha                90
_cell_angle_beta                 105.394(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.4262(5)
_cell_length_b                   16.3000(3)
_cell_length_c                   39.968(3)
_cell_measurement_reflns_used    95210
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     15342.2(13)
_computing_cell_refinement       'LaueG (Piltz, 2011)'
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)'
_computing_molecular_graphics    various
_computing_publication_material
;
CRYSTALS + LaueG  (Piltz 2011)
;
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.768
_diffrn_measured_fraction_theta_max 0.768
_diffrn_measurement_details
;
11 images in 2 settings, exposure time 5000 seconds
;
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.85
_diffrn_reflns_av_R_equivalents  0.5023
_diffrn_reflns_av_unetI/netI     0.5278
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            48674
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.11
_diffrn_reflns_theta_full        69.95
_diffrn_reflns_theta_max         70.05
_diffrn_reflns_theta_min         3.350
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_source_type
'OPAL reactor, ANSTO, Lucas Heights, Australia'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.798
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          1.50
_exptl_crystal_size_mid          1.0
_exptl_crystal_size_min          0.8
_refine_diff_density_max         1.66
_refine_diff_density_min         -1.80
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1458
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         3158
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.2905
_refine_ls_R_factor_gt           0.1695
_refine_ls_shift/su_max          0.0000860
_refine_ls_shift/su_mean         0.0000109
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 12.2 7.09 -6.27 12.1 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2949
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1149
_reflns_limit_h_max              25
_reflns_limit_h_min              -27
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              44
_reflns_limit_l_min              0
_reflns_number_gt                4173
_reflns_number_total             8466
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1223
_oxford_refine_ls_scale          0.2518(17)
_oxford_reflns_number_all        8215
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title
'spider-15004 in D:\laueg\aje\haz At 14:12 on'
_cod_data_source_file            ic5b02073_si_002.cif
_cod_data_source_block           '_(CyPSiP)PtH_Neutron'
_cod_depositor_comments
'Adding full bibliography for 4344446--4344451.cif.'
_cod_original_cell_volume        15342.2(12)
_cod_original_sg_symbol_H-M      'C  2/c  '
_cod_original_formula_sum        'C79 H124.00 P4 Pt2 Si2'
_cod_database_code               4344451