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_7701117
_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         'C20 H21 Fe N9, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C22 H24 B2 F8 Fe N10'
_chemical_formula_weight         657.98
_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             2018-09-19
_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                68.952(6)
_cell_angle_beta                 84.954(6)
_cell_angle_gamma                63.988(7)
_cell_formula_units_Z            2
_cell_length_a                   10.9070(7)
_cell_length_b                   11.7927(7)
_cell_length_c                   12.8472(8)
_cell_measurement_reflns_used    7890
_cell_measurement_temperature    103.70(10)
_cell_measurement_theta_max      69.1340
_cell_measurement_theta_min      3.6290
_cell_volume                     1381.20(18)
_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_environment      N~2~
_diffrn_ambient_temperature      103.70(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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   -115.00 -14.00   1.00    4.50    --  -42.08 -57.00  30.00  101
  2  \w    -70.00  31.00   1.00    4.50    --  -42.08  57.00-180.00  101
  3  \w      1.00  83.00   1.00    4.50    --   42.08 -99.00 -90.00   82
  4  \w    -32.00  66.00   1.00    4.50    --   42.08 -37.00-120.00   98
  5  \w     94.00 173.00   1.00   18.00    --  100.00 125.00-150.00   79
  6  \w     17.00 109.00   1.00   18.00    --  100.00 -94.00   0.00   92
  7  \w     17.00 109.00   1.00   18.00    --  100.00 -94.00 120.00   92
  8  \w     71.00 172.00   1.00   18.00    --  100.00  61.00 -90.00  101
  9  \w     67.00 176.00   1.00   18.00    --  100.00  77.00 150.00  109
 10  \w     94.00 173.00   1.00   18.00    --  100.00 125.00 -30.00   79
 11  \w     27.00 121.00   1.00   18.00    --  100.00-125.00-120.00   94
 12  \w     27.00 121.00   1.00   18.00    --  100.00-125.00 -30.00   94
 13  \w     28.00 129.00   1.00   18.00    --  100.00 -61.00-150.00  101
 14  \w     71.00 172.00   1.00   18.00    --  100.00  61.00 -60.00  101
 15  \w     17.00 109.00   1.00   18.00    --  100.00 -94.00  30.00   92
 16  \w     67.00 176.00   1.00   18.00    --  100.00  77.00  30.00  109
 17  \w   -118.00  -9.00   1.00    4.50    --  -42.08 -77.00 150.00  109
 18  \w    -66.00  32.00   1.00    4.50    --  -42.08  37.00  90.00   98
 19  \w   -118.00  -9.00   1.00    4.50    --  -42.08 -77.00-120.00  109
 20  \w   -118.00  -9.00   1.00    4.50    --  -42.08 -77.00 -30.00  109
 21  \w   -115.00 -14.00   1.00    4.50    --  -42.08 -57.00 120.00  101
 22  \w     71.00 172.00   1.00   18.00    --  100.00  61.00-150.00  101
 23  \w     67.00 176.00   1.00   18.00    --  100.00  77.00 -60.00  109
 24  \w     71.00 172.00   1.00   18.00    --  100.00  61.00  90.00  101
 25  \w     67.00 143.00   1.00   18.00    --  100.00  77.00   0.00   76
;
_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      -0.1238794000
_diffrn_orient_matrix_UB_12      0.1220334000
_diffrn_orient_matrix_UB_13      0.0144494000
_diffrn_orient_matrix_UB_21      -0.0605716000
_diffrn_orient_matrix_UB_22      -0.0949702000
_diffrn_orient_matrix_UB_23      0.0743995000
_diffrn_orient_matrix_UB_31      0.0765324000
_diffrn_orient_matrix_UB_32      -0.0180773000
_diffrn_orient_matrix_UB_33      0.1043033000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19310
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        71.616
_diffrn_reflns_theta_max         71.616
_diffrn_reflns_theta_min         3.699
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.183
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.406
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0884P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4267
_reflns_number_total             5224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02829c2.cif
_cod_data_source_block           1_CH3CN_100K
_cod_depositor_comments
'Adding full bibliography for 7701117--7701119.cif.'
_cod_original_cell_volume        1381.19(17)
_cod_database_code               7701117
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Fe C22 H24 N10 B2 F8'
_reflns_odcompleteness_completeness 99.90
_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.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16)
2.d Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C20(H20a,H20b,H20c), C22(H22a,H22b,H22c)
;
_olex2_date_sample_submission    2018-09-18
_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 5.163
_oxdiff_exptl_absorpt_empirical_full_min 0.536