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_7219380
_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_sum            'C59 H80 Fe O2 P4'
_chemical_formula_weight         1000.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-12-14 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.067(4)
_cell_length_b                   12.873(3)
_cell_length_c                   22.808(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5598(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.1157
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31954
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.423
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2144
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         12629
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0770P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                6628
_reflns_number_total             12629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra00072f2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5598.0(19)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7219380