Insertion chemistry of iron(ii) boryl complexes
Narro, Ana L.; Arman, Hadi D.; Tonzetich, Zachary J.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02879D

data_7711349
_publ_section_title
;
 Insertion chemistry of iron(ii) boryl complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02879D
_journal_year                    2022
_chemical_formula_moiety         '8(C47 H77 B Fe N2 O2 P2), 3(C7 H14)'
_chemical_formula_sum            'C397 H658 B8 Fe8 N16 O16 P16'
_chemical_formula_weight         6940.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-02 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.24130(10)
_cell_length_b                   28.8530(2)
_cell_length_c                   34.7308(3)
_cell_measurement_reflns_used    47040
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.4380
_cell_measurement_theta_min      1.9950
_cell_volume                     11117.46(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.960
_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    -33.00  27.80   0.38   13.00    --  -46.78  24.00-109.00  160
  2  \w   -164.00 -85.72   0.38   51.99    --  -91.75-101.00 -42.00  206
  3  \w     77.00 162.88   0.38   51.99    --  106.90 152.00 118.00  226
  4  \w     93.00 177.36   0.38   51.99    --  106.90  24.00-109.00  222
  5  \w   -120.00 -84.28   0.38   13.00    --  -46.78 -57.00 -60.00   94
  6  \w    -43.00  26.16   0.38   13.00    --  -46.78  37.00   0.00  182
  7  \w     32.00  92.80   0.38   13.00    --   46.78-121.00-124.00  160
  8  \w     83.00 118.72   0.38   13.00    --   46.78  57.00  90.00   94
  9  \w    -51.00 -19.84   0.38   51.99    --  -91.75  45.00-120.00   82
 10  \w    -51.00 -19.84   0.38   51.99    --  -91.75  45.00-150.00   82
 11  \w    -51.00 -19.84   0.38   51.99    --  -91.75  45.00   0.00   82
 12  \w     34.00  99.74   0.38   51.99    --  106.90 -77.00  30.00  173
 13  \w     34.00  69.72   0.38   51.99    --  106.90 -61.00  30.00   94
 14  \w   -121.00 -80.72   0.38   13.00    --  -46.78 -37.00 -30.00  106
 15  \w   -120.00 -84.28   0.38   13.00    --  -46.78 -57.00-150.00   94
 16  \w    -21.00   7.12   0.38   13.00    --  -46.89 101.00  60.00   74
 17  \w    -51.00 -25.92   0.38   51.99    --  -91.75  45.00  90.00   66
 18  \w    -51.00 -24.78   0.38   51.99    --  -91.75  45.00  60.00   69
 19  \w    -66.00 -37.88   0.38   51.99    --  -91.75  61.00 -30.00   74
 20  \w     41.00  67.22   0.38   51.99    --  106.92 -94.00-180.00   69
 21  \w     34.00  61.36   0.38   51.99    --  106.92 -61.00 -30.00   72
 22  \w     42.00  68.22   0.38   51.99    --  106.92 -61.00 -60.00   69
 23  \w     34.00  60.22   0.38   51.99    --  106.92 -61.00-120.00   69
 24  \w     34.00  59.08   0.38   51.99    --  106.92 -61.00-180.00   66
 25  \w     42.00  68.22   0.38   51.99    --  106.92 -61.00 120.00   69
 26  \w     75.00 100.08   0.38   51.99    --  106.92 -77.00-120.00   66
 27  \w     39.00  65.22   0.38   51.99    --  106.92 -77.00-120.00   69
 28  \w   -121.00 -33.22   0.38   13.00    --  -46.89 -37.00   0.00  231
 29  \w   -121.00 -33.22   0.38   13.00    --  -46.89 -37.00-180.00  231
 30  \w   -121.00 -54.88   0.38   13.00    --  -46.89 -37.00-120.00  174
 31  \w   -121.00 -33.22   0.38   13.00    --  -46.89 -37.00  90.00  231
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0629879000
_diffrn_orient_matrix_UB_12      0.0065835000
_diffrn_orient_matrix_UB_13      0.0424379000
_diffrn_orient_matrix_UB_21      -0.0057039000
_diffrn_orient_matrix_UB_22      -0.0526653000
_diffrn_orient_matrix_UB_23      0.0067403000
_diffrn_orient_matrix_UB_31      0.1236371000
_diffrn_orient_matrix_UB_32      -0.0057664000
_diffrn_orient_matrix_UB_33      -0.0131776000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            103159
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.995
_diffrn_reflns_theta_min         2.578
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.970
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_description       plate
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.057
_refine_diff_density_max         3.047
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         20256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0826
_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^)+(0.0100P)^2^+56.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17605
_reflns_number_total             20256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd_anav1
_cod_database_code               7711349
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe C H P N O B'
_chemical_oxdiff_usercomment     'Ana's sample'
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.702
_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. Others
 Fixed Sof: C90A(0.6) C94A(0.6) H94A(0.6) H94B(0.6) H94C(0.6) C99(0.75)
 H99(0.75) C92A(0.6) H92A(0.6) H92B(0.6) H92C(0.6) C97(0.75) H97A(0.75)
 H97B(0.75) C91A(0.6) H91A(0.6) H91B(0.6) H91C(0.6) C96(0.75) H96A(0.75)
 H96B(0.75) C95(0.75) H95A(0.75) H95B(0.75) H95C(0.75) C98(0.75) H98(0.75)
 C101(0.75) H10C(0.75) H10D(0.75) H10E(0.75) C100(0.75) H10F(0.75) H10G(0.75)
 C93A(0.6) H93A(0.6) H93B(0.6) H93C(0.6) C91B(0.4) H91D(0.4) H91E(0.4)
 H91F(0.4) C92B(0.4) H92D(0.4) H92E(0.4) H92F(0.4) C94B(0.4) H94D(0.4)
 H94E(0.4) H94F(0.4) C90B(0.4) C93B(0.4) H93D(0.4) H93E(0.4) H93F(0.4)
3.a Ternary CH refined with riding coordinates:
 C25(H25), C53(H53), C66(H66), C19(H19), C59(H59), C72(H72), C12(H12),
 C81(H81), C6(H6), C85(H85), C83(H83), C38(H38), C34(H34), C36(H36)
3.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C80(H80A,H80B), C30(H30A,H30B), C71(H71A,H71B), C58(H58A,
 H58B), C52(H52A,H52B), C18(H18A,H18B), C60(H60A,H60B), C65(H65A,H65B),
 C73(H73A,H73B), C70(H70A,H70B), C57(H57A,H57B), C86(H86A,H86B), C56(H56A,H56B),
  C29(H29A,H29B), C24(H24A,H24B), C5(H5A,H5B), C54(H54A,H54B), C28(H28A,H28B),
 C55(H55A,H55B), C14(H14A,H14B), C69(H69A,H69B), C20(H20A,H20B), C77(H77A,H77B),
  C74(H74A,H74B), C64(H64A,H64B), C13(H13A,H13B), C67(H67A,H67B), C21(H21A,
 H21B), C15(H15A,H15B), C7(H7A,H7B), C87(H87A,H87B), C76(H76A,H76B), C88(H88A,
 H88B), C26(H26A,H26B), C68(H68A,H68B), C11(H11A,H11B), C23(H23A,H23B),
 C17(H17A,H17B), C33(H33A,H33B), C75(H75A,H75B), C39(H39A,H39B), C84(H84A,H84B),
  C82(H82A,H82B), C16(H16A,H16B), C22(H22A,H22B), C27(H27A,H27B), C41(H41A,
 H41B), C37(H37A,H37B), C61(H61A,H61B), C35(H35A,H35B), C8(H8A,H8B), C9(H9A,
 H9B), C63(H63A,H63B), C62(H62A,H62B), C10(H10A,H10B), C97(H97A,H97B), C96(H96A,
 H96B), C100(H10F,H10G)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C50(H50), C49(H49), C99(H99), C98(H98)
3.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C94A(H94A,H94B,H94C), C92A(H92A,H92B,H92C), C91A(H91A,H91B,H91C),
 C95(H95A,H95B,H95C), C101(H10C,H10D,H10E), C93A(H93A,H93B,H93C), C91B(H91D,
 H91E,H91F), C92B(H92D,H92E,H92F), C94B(H94D,H94E,H94F), C93B(H93D,H93E,H93F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37988
_shelx_hkl_checksum              44029
_shelx_fab_checksum              72168
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.033
_oxdiff_exptl_absorpt_empirical_full_min 0.675