Synthesis of [POCOP]-Pincer Iron and Cobalt Complexes via Csp3-H Activation and Catalytic Application of Iron Hydride in Hydrosilylation Reactions
huang, shaofeng; zhao, hua; Li, Xiaoyan; wang, lin; Sun, Hongjian; RSC Adv.  (2015) –; doi:10.1039/C5RA00072F

data_7219383
_publ_section_title
;
 Synthesis of [POCOP]-Pincer Iron and Cobalt Complexes via Csp3-H
 Activation and Catalytic Application of Iron Hydride in Hydrosilylation
 Reactions
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA00072F
_journal_year                    2015
_chemical_formula_moiety         'C59 H80 Ni O2 P4'
_chemical_formula_sum            'C59 H80 Ni O2 P4'
_chemical_formula_weight         1003.82
_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   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-01-09 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                96.364(3)
_cell_angle_beta                 92.785(3)
_cell_angle_gamma                118.212(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2600(5)
_cell_length_b                   14.5978(6)
_cell_length_c                   15.3049(7)
_cell_measurement_reflns_used    16881
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.16
_cell_volume                     2771.6(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      ' 294 frames, detector distance = 130 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0938
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23118
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.688
_diffrn_reflns_theta_min         2.163
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.9638
_exptl_absorpt_correction_T_min  0.9013
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       rod
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0327P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6617
_reflns_number_total             10325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra00072f2.cif
_cod_data_source_block           D:\1alle\2013Li38\abskorr\2013-Li38
_cod_original_cell_volume        2771.5(2)
_cod_database_code               7219383
_shelxl_version_number           2013-2
_shelx_res_checksum              40666
_shelx_hkl_checksum              7540