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_7227832
_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 H50 Cl2 Fe N2'
_chemical_formula_sum            'C57 H50 Cl2 Fe N2'
_chemical_formula_weight         889.74
_chemical_name_common            (Dipp-BIANMe)FeCl2
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                98.172(2)
_cell_angle_beta                 99.125(2)
_cell_angle_gamma                99.657(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5987(3)
_cell_length_b                   12.0841(3)
_cell_length_c                   18.4864(5)
_cell_measurement_reflns_used    8849
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.9530
_cell_measurement_theta_min      4.2880
_cell_volume                     2269.67(11)
_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    'olex2.solve (Bourhis et al., 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 1.000
_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    -30.00  24.00   1.00    1.36    --  -41.89  37.00 120.00   54
  2  \w    -65.00 -34.00   1.00    1.36    --  -41.89  37.00 120.00   31
  3  \w   -116.00 -18.00   1.00    1.36    --  -41.89 -37.00 -60.00   98
  4  \w     58.00  92.00   1.00    1.36    --   41.89-125.00  30.00   34
  5  \w     84.00 120.00   1.00    5.47    --  107.79-125.00   0.00   36
  6  \w     50.00 140.00   1.00    5.47    --  107.79 -77.00 -30.00   90
  7  \w    151.00 177.00   1.00    5.47    --  107.79  30.00  30.00   26
  8  \w    120.00 146.00   1.00    5.47    --  107.79 125.00-120.00   26
  9  \w     95.00 153.00   1.00    5.47    --  107.79 125.00 -60.00   58
 10  \w     84.00 178.00   1.00    5.47    --  107.79  45.00   0.00   94
 11  \w     81.00 175.00   1.00    5.47    --  107.79  30.00 -60.00   94
 12  \w     41.00 100.00   1.00    5.47    --  107.79 -94.00-150.00   59
 13  \w     36.00 130.00   1.00    5.47    --  107.79 -61.00-150.00   94
 14  \w     36.00 120.00   1.00    5.47    --  107.79-125.00-180.00   84
 15  \w     32.00 133.00   1.00    5.47    --  107.79 -30.00 -30.00  101
 16  \w      4.00  71.00   1.00    1.36    --   41.89 -98.00 177.00   67
 17  \w   -116.00 -26.00   1.00    1.36    --  -41.89 -37.00-150.00   90
;
_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      0.1188618000
_diffrn_orient_matrix_UB_12      0.0807096000
_diffrn_orient_matrix_UB_13      0.0508424000
_diffrn_orient_matrix_UB_21      -0.0791594000
_diffrn_orient_matrix_UB_22      0.0127586000
_diffrn_orient_matrix_UB_23      0.0627239000
_diffrn_orient_matrix_UB_31      0.0461762000
_diffrn_orient_matrix_UB_32      -0.1027849000
_diffrn_orient_matrix_UB_33      0.0287289000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15165
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         3.768
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.052
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.646
_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    1.302
_exptl_crystal_description       needle
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         8269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0592P)^2^+0.4666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7547
_reflns_number_total             8269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra01511a2.cif
_cod_data_source_block           16120804
_cod_original_cell_volume        2269.69(10)
_cod_database_code               7227832
_chemical_oxdiff_formula         'C H N Fe Cl'
_chemical_oxdiff_usercomment     BIAN--FeCl2(-Me)
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C19(H19), C31(H31), C44(H44), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C8(H8), C6(H6), C9(H9), C15(H15), C5(H5), C17(H17),
 C16(H16), C50(H50), C27(H27), C43(H43), C46(H46), C56(H56), C29(H29), C53(H53),
  C52(H52), C41(H41), C54(H54), C34(H34), C33(H33), C49(H49), C48(H48),
 C40(H40), C47(H47), C39(H39), C55(H55), C37(H37), C36(H36), C42(H42), C35(H35)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C57(H57A,H57B,H57C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              82321
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.735