Pyridine N-oxide promoted hydrosilylation of carbonyl compounds catalyzed by [PSiP]-pincer iron hydrides.
Chang, Guoliang; Zhang, Peng; Yang, Wenjing; Xie, Shangqing; Sun, Hongjian; Li, Xiaoyan; Fuhr, Olaf; Fenske, Dieter; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9349–9354; doi:10.1039/d0dt00392a

data_7704679
_publ_section_title
;
 Pyridine N-oxide promoted hydrosilylation of carbonyl compounds catalyzed
 by [PSiP]-pincer iron hydrides.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9349
_journal_page_last               9354
_journal_paper_doi               10.1039/d0dt00392a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C48 H52 Fe P4 Si'
_chemical_formula_sum            'C48 H52 Fe P4 Si'
_chemical_formula_weight         836.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-18 deposited with the CCDC.	2020-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4493(2)
_cell_length_b                   21.2072(2)
_cell_length_c                   10.7787(3)
_cell_measurement_reflns_used    37567
_cell_measurement_temperature    180
_cell_measurement_theta_max      64.44
_cell_measurement_theta_min      2.08
_cell_volume                     4217.25(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      180.0
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            Dectris
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22903
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.497
_diffrn_reflns_theta_min         4.133
_exptl_absorpt_coefficient_mu    3.197
_exptl_absorpt_correction_T_max  0.6794
_exptl_absorpt_correction_T_min  0.1226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         5184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0441P)^2^+1.4036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4682
_reflns_number_total             5184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00392a2.cif
_cod_data_source_block           sun33
_cod_depositor_comments          'Adding full bibliography for 7704679.cif.'
_cod_database_code               7704679
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.418
_shelx_estimated_absorpt_t_min   0.401
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H23A(0.5) H23B(0.5) H23C(0.5)
3.a Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              47892
_olex2_submission_special_instructions 'No special instructions were received'