Variable coordination of tris(2-pyridyl)phosphine and its oxide toward M(hfac)2: a metal-specifiable switching between the formation of mono- and bis-scorpionate complexes
Artem'ev, Alexander; Kashevskii, Alexey; Bogomyakov, Artem Stepanovich; Safronov, Alexander; Sutyrina, Anastasiya Sutyrina; Telezhkin, Anton; Sterkhova, Irina; Dalton Trans.  (2017) –; doi:10.1039/C7DT00339K

data_7042626
_publ_section_title
;
 Variable coordination of tris(2-pyridyl)phosphine and its oxide toward
 M(hfac)2: a metal-specifiable switching between the formation of mono-
 and bis-scorpionate complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00339K
_journal_year                    2017
_chemical_formula_moiety         'C20 H15 F6 N3 Ni O4 P, C5 H F6 O2'
_chemical_formula_sum            'C25 H16 F12 N3 Ni O6 P'
_chemical_formula_weight         772.07
_chemical_melting_point          425
_chemical_name_systematic
'complex of tris(2-pyridyl)phosphine with nickel hexafluoroacetylacetonate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-14 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8330(8)
_cell_length_b                   15.6509(15)
_cell_length_c                   21.6876(17)
_cell_measurement_temperature    100(2)
_cell_volume                     2998.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            94343
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.112
_diffrn_reflns_theta_min         2.285
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 3085 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0298P)^2^+1.4075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7699
_reflns_number_total             8828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00339k2.cif
_cod_data_source_block           1
_cod_database_code               7042626
_shelx_estimated_absorpt_t_min   0.685
_shelx_estimated_absorpt_t_max   0.901
_shelxl_version_number           2013-3
_shelx_res_checksum              72452