Homoleptic Iron(II) and Cobalt(II) Bis (phosphoranimide) Complexes for Selective Hydrofunctionalization of Unsaturated Molecules
Bai, Tao; Janes, Trevor; Song, Datong; Dalton Trans.  (2017) –; doi:10.1039/C7DT02427D

data_7043943
_publ_section_title
;
 Homoleptic Iron(II) and Cobalt(II) Bis (phosphoranimide) Complexes for
 Selective Hydrofunctionalization of Unsaturated Molecules
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02427D
_journal_year                    2017
_chemical_formula_sum            'C49.5 H111.5 Fe2 N4 P4'
_chemical_formula_weight         998.51
_chemical_name_systematic        Fe(bis-phosphoranimide)
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-01-03 deposited with the CCDC.
2017-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                83.232(5)
_cell_angle_beta                 80.779(5)
_cell_angle_gamma                64.931(5)
_cell_formula_units_Z            2
_cell_length_a                   12.448(2)
_cell_length_b                   13.300(2)
_cell_length_c                   19.898(3)
_cell_measurement_reflns_used    38231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.95
_cell_volume                     2940.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38231
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1097
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         14386
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+6.5653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                11209
_reflns_number_total             14386
_reflns_threshold_expression     >2sigma(I)
_publcif_datablock.id            {5993cbbe-db49-46bc-853e-66ec1f671b2e}
_cod_data_source_file            c7dt02427d2.cif
_cod_data_source_block           tao3
_cod_original_cell_volume        2940.8(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C49.50 H111.50 Fe2 N4 P4'
_cod_database_code               7043943