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_4087745
_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         'C30 H42 N2 Ni O P2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C32 H45 B2 F8 N3 Ni O P2'
_chemical_formula_weight         781.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                92.4620(10)
_cell_angle_beta                 100.545(2)
_cell_angle_gamma                107.826(2)
_cell_formula_units_Z            4
_cell_length_a                   11.4094(4)
_cell_length_b                   11.4298(4)
_cell_length_c                   30.3230(12)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100
_cell_measurement_theta_max      78.70
_cell_measurement_theta_min      4.20
_cell_volume                     3680.2(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.11
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            70236
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.736
_diffrn_reflns_theta_min         2.981
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.208
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.6608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1031 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.8762.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.764
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         15503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+13.1986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12700
_reflns_number_total             15503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00562_si_011.cif
_cod_data_source_block           p15163
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C30 H42 N2 Ni O P2), 4(B F4), 2(C2 H3 N)'
_cod_original_formula_sum        'C64 H90 B4 F16 N6 Ni2 O2 P4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1563.95
_cod_database_code               4087745
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.608
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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), C18B(H18B), C21B(H21B), C24B(H24B),
 C27B(H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C3B(H3B), C4B(H4B), C8B(H8B), C9B(H9B), C10B(H10B),
 C11B(H11B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B)
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), C30(H30A,H30B,H30C), C19B(H19D,H19E,H19F), C20B(H20D,H20E,H20F),
 C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F), C25B(H25D,H25E,H25F), C26B(H26D,
 H26E,H26F), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F),
 C64(H64A,H64B,H64C), C64B(H64D,H64E,H64F)
;
_shelx_res_checksum              62882
_shelx_hkl_checksum              51991
_olex2_submission_special_instructions 'No special instructions were received'