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_7043944
_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            'C53 H120 Co2 N4 P4'
_chemical_formula_weight         1055.26
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-04-05 deposited with the CCDC.
2017-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1030(10)
_cell_length_b                   22.7743(10)
_cell_length_c                   22.3132(9)
_cell_measurement_reflns_used    172361
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.529
_cell_measurement_theta_min      2.834
_cell_volume                     12248.4(9)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            172361
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_min         2.834
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            deepgreen
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             4640
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6874
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.022(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         25317
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0454P)^2^+25.5976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                22219
_reflns_number_total             25317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02427d2.cif
_cod_data_source_block           tao5a
_cod_database_code               7043944
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.6874
_shelx_estimated_absorpt_t_max   0.7456
_shelx_res_checksum              31223