Tuning of Metal Complex Electronics and Reactivity by Remote Lewis Acid Binding to π-Coordinated Pyridine Diphosphine Ligands
Horak, Kyle T.; VanderVelde, David G.; Agapie, Theodor; Organometallics 34 (2015) 4753–; doi:10.1021/acs.organomet.5b00562

data_4087752
_publ_section_title
;
 Tuning of Metal Complex Electronics and Reactivity by Remote Lewis Acid
 Binding to \p-Coordinated Pyridine Diphosphine Ligands
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4753
_journal_paper_doi               10.1021/acs.organomet.5b00562
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C29 H40 N P2 Pd, C F3 O3 S'
_chemical_formula_sum            'C30 H40 F3 N O3 P2 Pd S'
_chemical_formula_weight         720.03
_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
_audit_creation_date             2015-05-06
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 102.437(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2515(8)
_cell_length_b                   11.1901(7)
_cell_length_c                   24.2291(15)
_cell_measurement_reflns_used    9621
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.49
_cell_volume                     3243.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            139953
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.570
_diffrn_reflns_theta_min         1.702
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0550 before and 0.0513 after correction. 
The Ratio of minimum to maximum transmission is 0.9404. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         9942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+1.6865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9135
_reflns_number_total             9942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00562_si_007.cif
_cod_data_source_block           a14122_0m
_cod_database_code               4087752
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All N(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Ternary CH refined with riding coordinates: 
 C18(H18), C21(H21), C24(H24), C27(H27) 
2.b Aromatic/amide H refined with riding coordinates: 
 N1(H1), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), 
 C17(H17) 
2.c Idealised Me refined as rotating group: 
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B, 
 H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A, 
 H29B,H29C) 
;
_shelx_res_checksum              68874
_shelx_hkl_checksum              53884
_olex2_submission_special_instructions 'No special instructions were received'