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_7227833
_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         'C60 H55 Cl2 F Fe N2 O, 2(C4 H8 O)'
_chemical_formula_sum            'C68 H71 Cl2 F Fe N2 O3'
_chemical_formula_weight         1110.01
_chemical_name_common            (Dipp-BIANF)FeCl2
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.38300(14)
_cell_length_b                   21.4869(4)
_cell_length_c                   25.4145(3)
_cell_measurement_reflns_used    13171
_cell_measurement_temperature    93
_cell_measurement_theta_max      77.2380
_cell_measurement_theta_min      3.4680
_cell_volume                     5669.94(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.40t (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_temperature      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_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   -122.00 -18.00   1.00    8.00    --  -32.00 -72.00-180.00  104
  2  \w    -57.00  24.00   1.00    8.00    --  -32.00   0.00-180.00   81
  3  \w   -178.00 -29.00   1.00   25.00    -- -110.00   0.00-108.00  149
  4  \w    -80.00 -20.00   1.00   25.00    -- -110.00  72.00 108.00   60
  5  \w    -80.00 -20.00   1.00   25.00    -- -110.00  72.00 -36.00   60
  6  \w   -125.00 -63.00   1.00   25.00    -- -110.00  72.00-180.00   62
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1013746000
_diffrn_orient_matrix_UB_12      0.0458496000
_diffrn_orient_matrix_UB_13      0.0213341000
_diffrn_orient_matrix_UB_21      0.0749117000
_diffrn_orient_matrix_UB_22      0.0546472000
_diffrn_orient_matrix_UB_23      -0.0245300000
_diffrn_orient_matrix_UB_31      -0.0782928000
_diffrn_orient_matrix_UB_32      -0.0070885000
_diffrn_orient_matrix_UB_33      -0.0511690000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17736
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.992
_diffrn_reflns_theta_min         2.693
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.414
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.40t (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.515(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         9426
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0600P)^2^+1.8850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                9046
_reflns_number_total             9426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra01511a2.cif
_cod_data_source_block           mzw_z_cu
_cod_original_cell_volume        5669.94(14)
_cod_database_code               7227833
_reflns_odcompleteness_completeness 94.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.34
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.485(4) 0.515(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C26-C31
 1.39 with sigma of 0.005
 C29-C28
 1.39 with sigma of 0.02
 C30-C29
 1.39 with sigma of 0.02
4. Rigid bond restraints
 C69, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C69 \\sim C68: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08
6. Same fragment restrains
{O3, C68, C67, C66, C65} sigma for 1-2: 0.02, 1-3: 0.04
{O3, C69, C67, C66, C65} sigma for 1-2: 0.02, 1-3: 0.04
as
{O3, C65, C66, C67, C68}
7. Others
 Sof(H67C)=Sof(H67D)=Sof(C69)=Sof(H69A)=Sof(H69B)=1-FVAR(1)
 Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=FVAR(1)
8.a Ternary CH refined with riding coordinates:
 C32(H32), C19(H19), C54(H54), C51(H51)
8.b Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C59(H59A,H59B), C57(H57A,H57B), C60(H60A,H60B), C61(H61A,
 H61B), C63(H63A,H63B), C62(H62A,H62B), C65(H65A,H65B), C66(H66A,H66B),
 C67(H67A,H67B), C67(H67C,H67D), C68(H68A,H68B), C69(H69A,H69B), C64(H64A,H64B)
8.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C17(H17), C5(H5), C3(H3), C11(H11), C10(H10), C15(H15), C9(H9),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C43(H43), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C40(H40), C44(H44), C41(H41), C35(H35),
 C34(H34), C38(H38), C42(H42), C36(H36), C37(H37), C47(H47), C48(H48), C49(H49)
8.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C53(H53A,H53B,H53C), C52(H52A,H52B,
 H52C)
;
_shelx_res_checksum              81357
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.937
_oxdiff_exptl_absorpt_empirical_full_min 0.640