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

data_7711348
_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         'C45 H69 B Fe N O2 P2'
_chemical_formula_sum            'C45 H69 B Fe N O2 P2'
_chemical_formula_weight         784.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-09-02 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.548(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.5218(11)
_cell_length_b                   10.8538(5)
_cell_length_c                   23.1258(8)
_cell_measurement_reflns_used    12789
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      72.7390
_cell_measurement_theta_min      2.4070
_cell_volume                     9163.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_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      99.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.950
_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    -83.00  -5.00   0.50   42.00    --  -46.62 114.00  39.00  156
  2  \w    -51.00 -17.00   0.50  168.00    --  -88.50  45.00   0.00   68
  3  \w    -46.00 -21.00   0.50  168.00    --  -88.50  45.00 -90.00   50
  4  \w    -45.00 -16.00   0.50  168.00    --  -88.50  45.00-150.00   58
  5  \w    -50.00 -18.00   0.50  168.00    --  -88.50  45.00-120.00   64
  6  \w    -51.00 -25.00   0.50  168.00    --  -88.50  45.00-180.00   52
  7  \w   -116.00 -35.00   0.50   42.00    --  -46.62 169.00-176.00  162
  8  \w    102.00 178.00   0.50  168.00    --  106.69 114.00  39.00  152
  9  \w    131.00 178.00   0.50  168.00    --  106.69  30.00-150.00   94
 10  \w     91.00 128.00   0.50  168.00    --  106.69  30.00-150.00   74
 11  \w     75.00 100.00   0.50  168.00    --  106.69 -77.00 -30.00   50
 12  \w     83.00 109.00   0.50  168.00    --  106.69-125.00   0.00   52
 13  \w     41.00  71.00   0.50  168.00    --  106.69 -61.00 -30.00   60
 14  \w     43.00  71.00   0.50  168.00    --  106.69 -77.00 -30.00   56
 15  \w     34.00 109.00   0.50  168.00    --  106.69-114.00 -50.00  150
 16  \w     40.00  76.00   0.50  168.00    --  106.69-125.00   0.00   72
 17  \w     34.00  59.00   0.50  168.00    --  106.69 -61.00   0.00   50
 18  \w     34.00  59.00   0.50  168.00    --  106.69 -61.00  90.00   50
 19  \w     42.00  68.00   0.50  168.00    --  106.69 -61.00 120.00   52
 20  \w     57.00 123.00   0.50   42.00    --   46.62-169.00 165.00  132
 21  \w     57.00 143.00   0.50  168.00    --  106.69-169.00 165.00  172
 22  \w     27.00  90.00   0.50   42.00    --   46.62-114.00 -50.00  126
 23  \w     35.00  61.00   0.50  168.00    --  106.69 -61.00-150.00   52
 24  \w     67.00 149.00   0.50  168.00    --  106.69 169.00-176.00  164
 25  \w    -70.00 -22.00   0.50  168.00    --  -88.50  61.00 150.00   96
 26  \w   -116.00 -84.00   0.50   42.00    --  -46.62 -57.00 -30.00   64
 27  \w   -114.00 -84.00   0.50   42.00    --  -46.62 -57.00 -60.00   60
 28  \w   -117.00 -85.00   0.50   42.00    --  -46.62 -57.00 -90.00   64
 29  \w   -112.00 -86.00   0.50   42.00    --  -46.62 -57.00-150.00   52
 30  \w   -116.00 -85.00   0.50   42.00    --  -46.62 -57.00-180.00   62
 31  \w   -160.00 -80.00   0.50  168.00    --  -88.50-114.00 -50.00  160
 32  \w   -119.00 -94.00   0.50   42.00    --  -46.62-125.00   0.00   50
 33  \w   -119.00 -45.00   0.50   42.00    --  -46.62-169.00 165.00  148
;
_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      -0.0023122000
_diffrn_orient_matrix_UB_12      -0.1392576000
_diffrn_orient_matrix_UB_13      0.0118698000
_diffrn_orient_matrix_UB_21      0.0295853000
_diffrn_orient_matrix_UB_22      0.0127750000
_diffrn_orient_matrix_UB_23      0.0483659000
_diffrn_orient_matrix_UB_31      -0.0299905000
_diffrn_orient_matrix_UB_32      0.0240372000
_diffrn_orient_matrix_UB_33      0.0443279000
_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  0.0908
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43546
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.541
_diffrn_reflns_theta_min         3.824
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.551
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
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    1.137
_exptl_crystal_description       plate
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         9146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0350P)^2^+51.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6881
_reflns_number_total             9146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd449e
_cod_database_code               7711348
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe C N H P'
_chemical_oxdiff_usercomment     'Ana Sample'
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.688
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C44B) = Uanis(C44A) = Uanis(C45B) = Uanis(C43B) = Uanis(C43A) =
Uanis(C45A)
3. Others
 Fixed Sof: H13A(0.6) H13B(0.6) H13C(0.4) H13D(0.4) H16A(0.6) H16B(0.6)
 H16C(0.4) H16D(0.4) H12A(0.4) H12(0.6) C44B(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
 C43B(0.5) C15B(0.6) H15A(0.6) H15B(0.6) C17B(0.6) H17B(0.6) C14A(0.6)
 H14A(0.6) H14B(0.6) C45B(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C42A(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5) C41A(0.5) H41A(0.5) H41B(0.5) H41C(0.5)
 C42B(0.5) H42D(0.5) H42E(0.5) H42F(0.5) C17A(0.4) H17A(0.4) C14B(0.4)
 H14C(0.4) H14D(0.4) C15A(0.4) H15C(0.4) H15D(0.4) C45A(0.5) H45D(0.5)
 H45E(0.5) H45F(0.5) C43A(0.5) C41B(0.5) H41D(0.5) H41E(0.5) H41F(0.5)
 C44A(0.5) H44D(0.5) H44E(0.5) H44F(0.5)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C25(H25), C6(H6), C12(H12A), C12(H12)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C29(H29A,H29B), C28(H28A,H28B), C26(H26A,
 H26B), C18(H18A,H18B), C24(H24A,H24B), C21(H21A,H21B), C27(H27A,H27B), C5(H5A,
 H5B), C22(H22A,H22B), C13(H13A,H13B), C13(H13C,H13D), C11(H11A,H11B), C23(H23A,
 H23B), C10(H10A,H10B), C7(H7A,H7B), C16(H16A,H16B), C16(H16C,H16D), C9(H9A,
 H9B), C8(H8A,H8B), C15B(H15A,H15B), C14A(H14A,H14B), C14B(H14C,H14D),
 C15A(H15C,H15D)
4.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C38(H38), C3(H3), C35(H35), C2(H2), C37(H37), C36(H36), C17B(H17B),
 C17A(H17A)
4.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C44B(H44A,H44B,H44C), C45B(H45A,H45B,H45C), C42A(H42A,
 H42B,H42C), C41A(H41A,H41B,H41C), C42B(H42D,H42E,H42F), C45A(H45D,H45E,H45F),
 C41B(H41D,H41E,H41F), C44A(H44D,H44E,H44F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84216
_shelx_hkl_checksum              44700
_shelx_fab_checksum              10963
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 4.959
_oxdiff_exptl_absorpt_empirical_full_min 0.436