gem-Dialkyl Effect in Diphosphine Ligands: Synthesis, Coordination Behavior, and Application in Pd-Catalyzed Hydroformylation
Tay, Dillon W. P.; Nobbs, James D.; Romain, Charles; White, Andrew J. P.; Aitipamula, Srinivasulu; van Meurs, Martin; Britovsek, George J. P.; ACS Catalysis 10 (2019) 663–; doi:10.1021/acscatal.9b03007

data_4517215
_publ_section_title
;
 gem-Dialkyl Effect in Diphosphine Ligands: Synthesis, Coordination
 Behavior, and Application in Pd-Catalyzed Hydroformylation
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              663
_journal_paper_doi               10.1021/acscatal.9b03007
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C35 H42 Cl2 P2 Pd, C H2 Cl2'
_chemical_formula_sum            'C36 H44 Cl4 P2 Pd'
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_space_group_name_Hall           '-P 2ac 2ab'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
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_diffrn_measured_fraction_theta_max 0.811
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -27
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_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_theta_min         2.448
_diffrn_source                   'Enhance (Mo) X-ray Source'
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_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.61
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00031(6)
_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   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7280
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0400P)^2^+21.5676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5500
_reflns_number_total             7280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b03007_si_002.cif
_cod_data_source_block           Pd-L3-Cl2
_cod_depositor_comments
'Adding full bibliography for 4517213--4517216.cif.'
_cod_database_code               4517215
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              79120
_shelx_hkl_checksum              8685