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_4087749
_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 H79 N2 Ni2 P4, C F3 O3 S, C6 H6'
_chemical_formula_sum            'C65 H85 F3 N2 Ni2 O3 P4 S'
_chemical_formula_weight         1272.71
_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   geom
_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                 99.777(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.003(3)
_cell_length_b                   13.924(2)
_cell_length_c                   22.832(4)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.33
_cell_volume                     6266.8(17)
_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 0.926
_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  0.0784
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84832
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.677
_diffrn_reflns_theta_min         1.720
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0616 before and 0.0571 after correction. 
The Ratio of minimum to maximum transmission is 0.8992. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         14952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0397P)^2^+3.4813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10238
_reflns_number_total             14952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00562_si_008.cif
_cod_data_source_block           a14150_0m
_cod_original_cell_volume        6267.1(18)
_cod_database_code               4087749
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.657
_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: 
 C50(H50), C30(H30), C56(H56), C53(H53), C47(H47), C1(H1), C18(H18), C21(H21), 
 C24(H24), C27(H27) 
2.b Aromatic/amide H refined with riding coordinates: 
 C4(H4), N2(H2), C33(H33), C32(H32), C46(H46), C45(H45), C44(H44), C43(H43), 
 C40(H40), C39(H39), C38(H38), C37(H37), C3(H3), C11(H11), C10(H10), C9(H9), 
 C8(H8), C14(H14), C15(H15), C16(H16), C17(H17), C63(H63), C62(H62), C61(H61), 
 C60(H60), C64(H64), C65(H65) 
2.c Idealised Me refined as rotating group: 
 C58(H58A,H58B,H58C), C55(H55A,H55B,H55C), C49(H49A,H49B,H49C), C52(H52A,H52B, 
 H52C), C51(H51A,H51B,H51C), C57(H57A,H57B,H57C), C54(H54A,H54B,H54C), C48(H48A, 
 H48B,H48C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), 
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C28(H28A,H28B, 
 H28C), C29(H29A,H29B,H29C) 
;
_shelx_res_checksum              90342
_shelx_hkl_checksum              73751
_olex2_submission_special_instructions 'No special instructions were received'