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_4087750
_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         'C58 H78 N2 Ni2 P4, C5 H12'
_chemical_formula_sum            'C63 H90 N2 Ni2 P4'
_chemical_formula_weight         1116.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-05-05
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 109.324(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7148(7)
_cell_length_b                   13.0646(5)
_cell_length_c                   25.9359(9)
_cell_measurement_reflns_used    9694
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.38
_cell_volume                     5984.1(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
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            63678
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.557
_diffrn_reflns_theta_min         1.630
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0489 before and 0.0431 after correction. 
The Ratio of minimum to maximum transmission is 0.9102. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         18228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0447P)^2^+2.3722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14315
_reflns_number_total             18228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00562_si_002.cif
_cod_data_source_block           a14144_0m
_cod_database_code               4087750
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.747
_shelx_estimated_absorpt_t_min   0.722
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 
2. Others 
 Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(C60B)= 
 Sof(H60C)=Sof(H60D)=Sof(C62B)=Sof(H62C)=Sof(H62D)=Sof(C61B)=Sof(H61C)= 
 Sof(H61D)=1-FVAR(1) 
 Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(C61A)= 
 Sof(H61A)=Sof(H61B)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C62A)=Sof(H62A)= 
 Sof(H62B)=FVAR(1) 
3.a Ternary CH refined with riding coordinates: 
 C53(H53), C56(H56), C47(H47), C50(H50), C21(H21), C18(H18), C24(H24), C27(H27) 
3.b Secondary CH2 refined with riding coordinates: 
 C60A(H60A,H60B), C61A(H61A,H61B), C62A(H62A,H62B), C60B(H60C,H60D), C62B(H62C, 
 H62D), C61B(H61C,H61D) 
3.c Me refined with riding coordinates: 
 C59(H59A,H59B,H59C), C59(H59D,H59E,H59F), C63(H63A,H63B,H63C), C63(H63D,H63E, 
 H63F) 
3.d Aromatic/amide H refined with riding coordinates: 
 C3(H3), C32(H32), C33(H33), C43(H43), C44(H44), C45(H45), C46(H46), C37(H37), 
 C38(H38), C39(H39), C40(H40), C4(H4), C11(H11), C10(H10), C9(H9), C8(H8), 
 C17(H17), C16(H16), C15(H15), C14(H14) 
3.e Idealised Me refined as rotating group: 
 C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C), C58(H58A,H58B, 
 H58C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A, 
 H52B,H52C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), 
 C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C29(H29A,H29B, 
 H29C), C28(H28A,H28B,H28C) 
;
_shelx_res_checksum              36957
_shelx_hkl_checksum              50067
_olex2_submission_special_instructions 'No special instructions were received'