Iron(ii) tetrafluoroborate complexes of new tetradentate C-scorpionates as catalysts for the oxidative cleavage of trans-stilbene with H<sub>2</sub>O<sub>2</sub>.
Wang, Denan; Gardinier, James R.; Lindeman, Sergey V.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14478–14489; doi:10.1039/c9dt02829c

data_7701118
_publ_section_title
;
 Iron(ii) tetrafluoroborate complexes of new tetradentate C-scorpionates
 as catalysts for the oxidative cleavage of trans-stilbene with
 H<sub>2</sub>O<sub>2</sub>.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14478
_journal_page_last               14489
_journal_paper_doi               10.1039/c9dt02829c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C24 H29 Fe N9, 0.33(C4 H10 O), 0.34(C2 H3 N), 2(B F4)'
_chemical_formula_sum            'C25.98 H33.28 B2 F8 Fe N9.34 O0.33'
_chemical_formula_weight         711.16
_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     iterative
_audit_creation_date             2018-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-03 deposited with the CCDC.    2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4179(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1371(3)
_cell_length_b                   12.73175(16)
_cell_length_c                   25.9506(4)
_cell_measurement_reflns_used    28694
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.6450
_cell_measurement_theta_min      4.2040
_cell_volume                     6381.95(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -71.00  31.00   1.00    7.50    --  -42.46  57.00  90.00  102
  2  \w   -117.00 -18.00   1.00    7.50    --  -42.46 -37.00 -60.00   99
  3  \w   -115.00 -14.00   1.00    7.50    --  -42.46 -57.00-120.00  101
  4  \w     74.00 173.00   1.00   30.00    --  100.00  45.00-150.00   99
  5  \w     27.00 121.00   1.00   30.00    --  100.00-125.00  30.00   94
  6  \w     28.00 129.00   1.00   30.00    --  100.00 -61.00 -90.00  101
  7  \w     94.00 173.00   1.00   30.00    --  100.00 125.00-150.00   79
  8  \w     17.00 109.00   1.00   30.00    --  100.00 -94.00  60.00   92
  9  \w     18.00 153.00   1.00   30.00    --  100.00 -15.00-150.00  135
 10  \w   -115.00 -65.00   1.00    7.50    --  -42.46-138.00  68.00   50
 11  \w   -119.00 -10.00   1.00    7.50    --  -42.46 -77.00  90.00  109
 12  \w     23.00  98.00   1.00    7.50    --   42.46-125.00 -60.00   75
 13  \w     24.00 133.00   1.00   30.00    --  100.00 -77.00 150.00  109
 14  \w     71.00 172.00   1.00   30.00    --  100.00  61.00 -60.00  101
 15  \w     71.00 127.00   1.00   30.00    --  100.00  61.00  60.00   56
 16  \w     71.00 172.00   1.00   30.00    --  100.00  61.00   0.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0719985000
_diffrn_orient_matrix_UB_12      -0.0113351000
_diffrn_orient_matrix_UB_13      0.0091613000
_diffrn_orient_matrix_UB_21      -0.0339071000
_diffrn_orient_matrix_UB_22      0.0053256000
_diffrn_orient_matrix_UB_23      -0.0611083000
_diffrn_orient_matrix_UB_31      0.0052303000
_diffrn_orient_matrix_UB_32      -0.1203298000
_diffrn_orient_matrix_UB_33      -0.0035785000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            60864
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        70.688
_diffrn_reflns_theta_max         70.688
_diffrn_reflns_theta_min         3.551
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.530
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.228
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       needle
_exptl_crystal_F_000             2921
_exptl_crystal_size_max          0.547
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.050
_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     911
_refine_ls_number_reflns         12132
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+4.7782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11351
_reflns_number_total             12132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02829c2.cif
_cod_data_source_block           2_0p3ACN_0p3Et2O
_cod_depositor_comments
'Adding full bibliography for 7701117--7701119.cif.'
_cod_original_cell_volume        6381.93(16)
_cod_database_code               7701118
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C24 H29 B2 F8 Fe N9'
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N1S, C1S, C2S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2S, C7S, C8S
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(O1S)=Sof(C3S)=Sof(H3SB)=Sof(H3SA)=Sof(C4S)=Sof(H4SA)=Sof(H4SC)=Sof(H4SB)=
 Sof(C5S)=Sof(H5SB)=Sof(H5SA)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=FVAR(1)
 Sof(N1S)=Sof(C1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=FVAR(2)
 Sof(N2S)=Sof(C7S)=Sof(C8S)=Sof(H8SA)=Sof(H8SB)=Sof(H8SC)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C15A(H15C,H15D), C3S(H3SB,H3SA), C5S(H5SB,H5SA)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C9(H9), C17(H17), C18(H18), C19(H19), C20(H20),
 C3A(H3A), C4A(H4A), C6A(H6A), C9A(H9A), C17A(H17A), C18A(H18A), C19A(H19A),
 C20A(H20A)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C11A(H11D,H11E,H11F),
 C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C22A(H22D,
 H22E,H22F), C24A(H24D,H24E,H24F), C4S(H4SA,H4SC,H4SB), C6S(H6SA,H6SB,H6SC),
 C8S(H8SA,H8SB,H8SC), C2S(H2SA,H2SB,H2SC)
;
_olex2_date_sample_data_collection 2018-10-16
_olex2_date_sample_submission    2018-10-15
_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 1.424
_oxdiff_exptl_absorpt_empirical_full_min 0.770