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_7042627
_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
'2(C15 H3 F18 Mn O6), C30 H24 Mn N6 P2, 2(C3 H6 O)'
_chemical_formula_sum            'C66 H42 F36 Mn3 N6 O14 P2'
_chemical_formula_weight         2053.82
_chemical_melting_point          490
_chemical_name_systematic
'complex of tris(2-pyridyl)phosphine with manganese hexafluoroacetylacetonate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                80.785(3)
_cell_angle_beta                 79.387(3)
_cell_angle_gamma                65.580(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5909(7)
_cell_length_b                   12.6726(9)
_cell_length_c                   16.6408(11)
_cell_measurement_temperature    100(2)
_cell_volume                     1990.0(2)
_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 0.995
_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  0.0770
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            123437
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.113
_diffrn_reflns_theta_min         2.263
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1021
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.071
_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     663
_refine_ls_number_reflns         11664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0336P)^2^+1.7612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8533
_reflns_number_total             11664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00339k2.cif
_cod_data_source_block           mo_Artemev_Mn_181114_0m
_cod_database_code               7042627
_shelx_estimated_absorpt_t_min   0.644
_shelx_estimated_absorpt_t_max   0.761
_shelxl_version_number           2013-3
_shelx_res_checksum              13586