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_7227836
_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         'C54 H44 Cl2 Fe N2, C58 H52 Cl2 Fe N2 O'
_chemical_formula_sum            'C112 H96 Cl4 Fe2 N4 O'
_chemical_formula_weight         1767.42
_chemical_name_common            (Mes-BIANMe)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
_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                 102.115(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7651(4)
_cell_length_b                   14.8041(3)
_cell_length_c                   34.0600(7)
_cell_measurement_reflns_used    19838
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.6270
_cell_measurement_theta_min      3.6030
_cell_volume                     9744.1(4)
_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    'ShelXT (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -28.00  82.00   1.00   71.78    --   13.10  19.00   0.00  110
  2  \w     38.00  63.00   1.00   71.78    --   13.10  38.00 -90.00   25
  3  \w      0.00  34.00   1.00   71.78    --   13.10  71.00  44.00   34
  4  \w    -52.00 -27.00   1.00   71.78    --   13.10 -57.00-180.00   25
  5  \w     49.00 100.00   1.00   71.78    --   13.10-178.00-180.00   51
  6  \w     40.00  73.00   1.00   71.78    --   13.10-178.00-150.00   33
;
_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      -0.0053726000
_diffrn_orient_matrix_UB_12      0.0359772000
_diffrn_orient_matrix_UB_13      -0.0140693000
_diffrn_orient_matrix_UB_21      0.0298934000
_diffrn_orient_matrix_UB_22      -0.0133200000
_diffrn_orient_matrix_UB_23      -0.0069657000
_diffrn_orient_matrix_UB_31      -0.0205990000
_diffrn_orient_matrix_UB_32      -0.0287002000
_diffrn_orient_matrix_UB_33      -0.0143987000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            63916
_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         25.998
_diffrn_reflns_theta_min         3.275
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       plate
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         19110
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0732P)^2^+10.5613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12508
_reflns_number_total             19110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra01511a2.cif
_cod_data_source_block           16120703_sq
_cod_original_cell_volume        9744.1(3)
_cod_database_code               7227836
_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. Rigid bond restraints
 O1, Fe2, C112, C109, C110, C111
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Fe2 \\sim O1 \\sim C109 \\sim C110 \\sim C111 \\sim C112: within 1.7A with
sigma of 0.005 and sigma for terminal atoms of 0.08
Uanis(Cl5) = Uanis(Cl3)
Uanis(Fe3) = Uanis(Fe2)
4. Same fragment restrains
{O1, C112, C111, C110, C109} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1, C109, C110, C111, C112}
5. Others
 Sof(Fe3)=Sof(Cl5)=1-FVAR(1)
 Sof(Fe2)=Sof(Cl3)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C44(H44), C82(H82), C96(H96)
6.b Secondary CH2 refined with riding coordinates:
 C109(H10A,H10B), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C16(H16), C9(H9), C8(H8), C17(H17), C5(H5), C6(H6), C4(H4),
 C18(H18), C21(H21), C22(H22), C20(H20), C43(H43), C53(H53), C52(H52), C33(H33),
  C50(H50), C42(H42), C27(H27), C41(H41), C56(H56), C49(H49), C46(H46),
 C29(H29), C39(H39), C40(H40), C36(H36), C34(H34), C37(H37), C35(H35), C48(H48),
  C47(H47), C54(H54), C55(H55), C61(H61), C59(H59), C78(H78), C69(H69),
 C71(H71), C80(H80), C84(H84), C108(H108), C94(H94), C90(H90), C88(H88),
 C85(H85), C104(H104), C98(H98), C92(H92), C102(H102), C93(H93), C86(H86),
 C107(H107), C91(H91), C87(H87), C99(H99), C105(H105), C106(H106), C101(H101),
 C100(H100)
6.d Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C64(H64A,H64B,H64C), C63(H63A,H63B,
 H63C), C75(H75A,H75B,H75C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C95(H95A,
 H95B,H95C)
;
_shelx_res_checksum              24037
_shelx_fab_checksum              78614
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'