Ferrous complexes supported by sterically encumbered asymmetric bis(arylimino)acenaphthene (BIAN) ligands: synthesis, characterization and screening for catalytic hydrosilylation of carbonyl compounds
Yu, Xun; Zhu, Feifeng; Bu, Donglei; Lei, Hao; RSC Adv. 7 (2017) 15321–; doi:10.1039/C7RA01511A

data_7227834
_publ_section_title
;
 Ferrous complexes supported by sterically encumbered asymmetric
 bis(arylimino)acenaphthene (BIAN) ligands: synthesis, characterization
 and screening for catalytic hydrosilylation of carbonyl compounds
;
_journal_issue                   25
_journal_name_full               'RSC Adv.'
_journal_page_first              15321
_journal_paper_doi               10.1039/C7RA01511A
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C57 H49 Cl3 Fe N2 O'
_chemical_formula_sum            'C57 H49 Cl3 Fe N2 O'
_chemical_formula_weight         940.18
_chemical_name_common            (Mes-BIANCl)FeCl2
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-03 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.5203(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.01587(18)
_cell_length_b                   14.80189(15)
_cell_length_c                   16.80964(17)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.0540
_cell_measurement_theta_min      3.9820
_cell_volume                     4600.30(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     23.00  64.00   1.00    1.02    --   41.89 -37.00 -60.00   41
  2  \w     27.00  95.00   1.00    4.08    --  108.44 -94.00-180.00   68
  3  \w     80.00 108.00   1.00    4.08    --  108.44 -94.00-150.00   28
  4  \w     36.00 128.00   1.00    4.08    --  108.44 -45.00-180.00   92
  5  \w    103.00 153.00   1.00    4.08    --  108.44  96.00 -90.00   50
  6  \w    101.00 126.00   1.00    4.08    --  108.44 -61.00 150.00   25
  7  \w     58.00  94.00   1.00    4.08    --  108.44 -94.00  60.00   36
  8  \w     28.00  54.00   1.00    4.08    --  108.44 -94.00  60.00   26
  9  \w     26.00 168.00   1.00    4.08    --  108.44   0.00  90.00  142
 10  \w    -33.00  -7.00   1.00    1.02    --   41.89 -37.00 -60.00   26
 11  \w   -115.00 -14.00   1.00    1.02    --  -41.89 -57.00  90.00  101
 12  \w    -79.00  -2.00   1.00    1.02    --  -41.89 125.00-180.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0012736000
_diffrn_orient_matrix_UB_12      0.0802297000
_diffrn_orient_matrix_UB_13      0.0586739000
_diffrn_orient_matrix_UB_21      0.0450038000
_diffrn_orient_matrix_UB_22      0.0551268000
_diffrn_orient_matrix_UB_23      -0.0480488000
_diffrn_orient_matrix_UB_31      -0.0701195000
_diffrn_orient_matrix_UB_32      0.0368705000
_diffrn_orient_matrix_UB_33      -0.0559440000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17968
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.983
_diffrn_reflns_theta_min         3.825
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.567
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_correction_T_min  0.168
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       prism
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.181
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         8354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0771
_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^)+(0.1320P)^2^+0.3630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7685
_reflns_number_total             8354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra01511a2.cif
_cod_data_source_block           16120803
_cod_database_code               7227834
_chemical_oxdiff_formula         'C H N Fe Cl'
_chemical_oxdiff_usercomment     BIAN--FeCl2(-Cl)
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C54(H54A,H54B), C56(H56A,H56B), C55(H55A,H55B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C28(H28), C3(H3), C42(H42), C47(H47), C11(H11), C32(H32), C22(H22),
 C38(H38), C26(H26), C13(H13), C15(H15), C29(H29), C36(H36), C41(H41), C19(H19),
  C18(H18), C49(H49), C37(H37), C40(H40), C24(H24), C25(H25), C30(H30),
 C31(H31), C12(H12), C9(H9), C10(H10), C17(H17), C23(H23), C16(H16)
2.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              3936
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.675
_oxdiff_exptl_absorpt_empirical_full_min 0.667