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_7227835
_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         'C53 H41 Cl2 F Fe N2'
_chemical_formula_sum            'C53 H41 Cl2 F Fe N2'
_chemical_formula_weight         851.63
_chemical_name_common            (Mes-BIANF)FeCl2
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.3046(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.87969(13)
_cell_length_b                   16.89054(15)
_cell_length_c                   18.35276(16)
_cell_measurement_reflns_used    9116
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.9090
_cell_measurement_theta_min      3.5830
_cell_volume                     4187.06(7)
_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 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    -75.00  -4.00   1.00    1.03    --  -41.89 125.00-120.00   71
  2  \w   -118.00  -9.00   1.00    1.03    --  -41.89 -77.00-180.00  109
  3  \w     48.00  93.00   1.00    1.03    --   41.89-125.00  60.00   45
  4  \w     84.00 122.00   1.00    4.10    --  107.79-125.00 120.00   38
  5  \w     78.00 133.00   1.00    4.10    --  107.79 -45.00  90.00   55
  6  \w     74.00 133.00   1.00    4.10    --  107.79 -45.00 150.00   59
  7  \w     82.00 171.00   1.00    4.10    --  107.79  45.00  90.00   89
  8  \w     85.00 178.00   1.00    4.10    --  107.79  45.00 -30.00   93
  9  \w    106.00 173.00   1.00    4.10    --  107.79 125.00 -90.00   67
 10  \w     74.00 105.00   1.00    4.10    --  107.79 -94.00 -60.00   31
;
_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      -0.1079634000
_diffrn_orient_matrix_UB_12      0.0082835000
_diffrn_orient_matrix_UB_13      0.0071554000
_diffrn_orient_matrix_UB_21      -0.0356158000
_diffrn_orient_matrix_UB_22      -0.0452760000
_diffrn_orient_matrix_UB_23      -0.0741966000
_diffrn_orient_matrix_UB_31      0.0090633000
_diffrn_orient_matrix_UB_32      -0.0787574000
_diffrn_orient_matrix_UB_33      0.0433911000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15648
_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         67.998
_diffrn_reflns_theta_min         3.602
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.406
_exptl_absorpt_correction_T_max  0.267
_exptl_absorpt_correction_T_min  0.256
_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    1.351
_exptl_crystal_description       prism
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0660P)^2^+1.4510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7143
_reflns_number_total             7619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra01511a2.cif
_cod_data_source_block           16120801
_cod_database_code               7227835
_chemical_oxdiff_formula         'C H N O Fe Cl F'
_chemical_oxdiff_usercomment     BIAN-FeCl2(-F)
_reflns_odcompleteness_completeness 99.95
_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:
 C28(H28), C41(H41)
2.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C49(H49), C4(H4), C45(H45), C51(H51), C8(H8), C53(H53), C9(H9),
 C31(H31), C43(H43), C46(H46), C5(H5), C32(H32), C40(H40), C50(H50), C6(H6),
 C37(H37), C39(H39), C47(H47), C33(H33), C30(H30), C15(H15), C10(H10), C34(H34),
  C26(H26), C38(H38), C24(H24), C52(H52), C17(H17), C44(H44)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              58969
_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 2.750
_oxdiff_exptl_absorpt_empirical_full_min 0.550