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_7227837
_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         'C56 H47 Cl3 Fe N2, C4 H8 O'
_chemical_formula_sum            'C60 H55 Cl3 Fe N2 O'
_chemical_formula_weight         982.26
_chemical_name_common            (Dipp-BIANCl)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                 96.4438(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.51517(14)
_cell_length_b                   18.6075(3)
_cell_length_c                   26.0044(3)
_cell_measurement_reflns_used    13155
_cell_measurement_temperature    93
_cell_measurement_theta_max      77.3260
_cell_measurement_theta_min      2.3630
_cell_volume                     5055.90(12)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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   -108.00  27.00   1.00    8.00    --  -32.00   0.00-180.00  135
  2  \w    -78.00 -18.00   1.00    8.00    --  -32.00 -72.00-180.00   60
  3  \w    -78.00 -18.00   1.00    8.00    --  -32.00 -72.00 108.00   60
  4  \w    -78.00  58.00   1.00    8.00    --  -32.00   0.00-108.00  136
  5  \w    -46.00  15.00   1.00    8.00    --  -32.00  72.00 108.00   61
  6  \w   -200.00 -20.00   1.00   25.00    -- -110.00   0.00-108.00  180
  7  \w    -98.00 -20.00   1.00   25.00    -- -110.00  72.00-180.00   78
  8  \w    -80.00 -20.00   1.00   25.00    -- -110.00  72.00 108.00   60
  9  \w    -80.00 -20.00   1.00   25.00    -- -110.00  72.00  36.00   60
 10  \w   -122.00-114.00   1.00   25.00    -- -110.00  72.00 -36.00    8
;
_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      0.0884666000
_diffrn_orient_matrix_UB_12      -0.0473101000
_diffrn_orient_matrix_UB_13      0.0371779000
_diffrn_orient_matrix_UB_21      0.0065394000
_diffrn_orient_matrix_UB_22      0.0597821000
_diffrn_orient_matrix_UB_23      0.0411771000
_diffrn_orient_matrix_UB_31      -0.1177589000
_diffrn_orient_matrix_UB_32      -0.0322558000
_diffrn_orient_matrix_UB_33      0.0218598000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23671
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         2.926
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.177
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.499
_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    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9019
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0700P)^2^+1.1170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7628
_reflns_number_total             9019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra01511a2.cif
_cod_data_source_block           mzw_cl_cu
_cod_original_cell_volume        5055.91(12)
_cod_database_code               7227837
_reflns_odcompleteness_completeness 92.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.50
_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. Same fragment restrains
{O1, C60, C59, C58, C57} sigma for 1-2: 0.001, 1-3: 0.04
as
{O1, C57, C58, C59, C60}
3.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C31(H31), C44(H44)
3.b Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C5(H5), C18(H18), C22(H22), C20(H20), C4(H4), C21(H21),
 C3(H3), C27(H27), C29(H29), C39(H39), C43(H43), C33(H33), C40(H40), C36(H36),
 C41(H41), C37(H37), C35(H35), C42(H42), C34(H34), C47(H47), C46(H46), C52(H52),
  C50(H50), C48(H48), C53(H53), C49(H49), C56(H56), C54(H54), C55(H55)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              22524
_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 2.070
_oxdiff_exptl_absorpt_empirical_full_min 0.678