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

data_7711343
_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         'C46 H63 Fe N3 O P2'
_chemical_formula_sum            'C46 H63 Fe N3 O P2'
_chemical_formula_weight         791.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2022-09-02 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                96.9410(10)
_cell_angle_beta                 105.4270(10)
_cell_angle_gamma                108.4270(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5389(2)
_cell_length_b                   13.3995(2)
_cell_length_c                   16.3112(3)
_cell_measurement_reflns_used    23729
_cell_measurement_temperature    99.97(18)
_cell_measurement_theta_max      75.9660
_cell_measurement_theta_min      2.8910
_cell_volume                     2053.00(7)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_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    -30.00  29.00   0.50    3.11    --  -46.75  19.00 -60.00  118
  2  \w    -51.00 -16.00   0.50   12.43    --  -88.50  45.00 -60.00   70
  3  \w    -51.00 -16.00   0.50   12.43    --  -88.50  45.00 -30.00   70
  4  \w    -51.00 -16.00   0.50   12.43    --  -88.50  45.00 -90.00   70
  5  \w    -84.00 -10.00   0.50    3.11    --  -46.75 121.00  -7.00  148
  6  \w    -71.00 -15.00   0.50   12.43    --  -88.50  61.00 120.00  112
  7  \w    -51.00 -16.00   0.50   12.43    --  -88.50  45.00 120.00   70
  8  \w    -84.00 -15.00   0.50   12.43    --  -88.50 121.00  -7.00  138
  9  \w   -104.00 -26.00   0.50    3.11    --  -46.75 151.00 153.00  156
 10  \w     83.00 119.00   0.50    3.11    --   46.75  57.00 -30.00   72
 11  \w     98.00 178.00   0.50   12.43    --  106.69 121.00  -7.00  160
 12  \w     95.00 178.00   0.50   12.43    --  106.69 125.00-150.00  166
 13  \w     95.00 178.00   0.50   12.43    --  106.69 125.00-120.00  166
 14  \w     95.00 178.00   0.50   12.43    --  106.69 125.00 -60.00  166
 15  \w     83.00 119.00   0.50    3.11    --   46.75  57.00 120.00   72
 16  \w     77.00 165.00   0.50   12.43    --  106.69 151.00 153.00  176
 17  \w    101.00 178.00   0.50   12.43    --  106.69  77.00 150.00  154
 18  \w     92.00 178.00   0.50   12.43    --  106.69  45.00 -30.00  172
 19  \w     32.00  94.00   0.50    3.11    --   46.75-121.00 -90.00  124
 20  \w     34.00 109.00   0.50   12.43    --  106.69-121.00 -90.00  150
 21  \w     47.00 128.00   0.50   12.43    --  106.69-148.00  49.21  162
 22  \w     48.00 111.00   0.50    3.11    --   46.75-151.00 109.00  126
 23  \w     48.00 129.00   0.50   12.43    --  106.69-151.00 109.00  162
 24  \w     34.00  71.00   0.50   12.43    --  106.69 -61.00 150.00   74
 25  \w     34.00 106.00   0.50   12.43    --  106.69 -98.00  83.89  144
 26  \w     44.00 125.00   0.50   12.43    --  106.69-143.00 -36.76  162
 27  \w     34.00  71.00   0.50   12.43    --  106.69 -61.00 120.00   74
 28  \w     34.00 105.00   0.50   12.43    --  106.69 -94.00  90.00  142
 29  \w     34.00 101.00   0.50   12.43    --  106.69 -77.00 -60.00  134
 30  \w     34.00 111.00   0.50   12.43    --  106.69-125.00-120.00  154
 31  \w     34.00 101.00   0.50   12.43    --  106.69 -77.00 -90.00  134
 32  \w   -104.00 -26.00   0.50   12.43    --  -88.50 151.00 153.00  156
 33  \w   -119.00 -32.00   0.50    3.11    --  -46.75 -48.00 -85.83  174
 34  \w   -119.00 -83.00   0.50    3.11    --  -46.75 -57.00 -60.00   72
 35  \w   -119.00 -31.00   0.50    3.11    --  -46.75 -52.00  16.16  176
 36  \w   -119.00 -55.00   0.50    3.11    --  -46.75-151.00 109.00  128
 37  \w   -119.00 -83.00   0.50    3.11    --  -46.75 -57.00 150.00   72
 38  \w   -119.00 -31.00   0.50    3.11    --  -46.75 -52.00  97.10  176
 39  \w   -119.00 -88.00   0.50    3.11    --  -46.75-125.00 -60.00   62
 40  \w   -119.00 -31.00   0.50    3.11    --  -46.75 -47.00-169.45  176
 41  \w   -119.00 -83.00   0.50    3.11    --  -46.75 -57.00-180.00   72
 42  \w   -160.00 -76.00   0.50   12.43    --  -88.50-121.00 -90.00  168
 43  \w   -119.00 -83.00   0.50    3.11    --  -46.75 -57.00  60.00   72
 44  \w   -119.00 -79.00   0.50    3.11    --  -46.75 -52.00 152.04   80
 45  \w   -148.00 -55.00   0.50   12.43    --  -88.50-151.00 109.00  186
 46  \w   -160.00 -91.00   0.50   12.43    --  -88.50 -61.00   0.00  138
 47  \w   -160.00 -91.00   0.50   12.43    --  -88.50 -61.00 -90.00  138
 48  \w   -160.00 -72.00   0.50   12.43    --  -88.50 -54.00 -23.84  176
 49  \w   -160.00-100.00   0.50   12.43    --  -88.50 -94.00 -30.00  120
 50  \w   -160.00-101.00   0.50   12.43    --  -88.50 -77.00 -60.00  118
;
_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      -0.0009102000
_diffrn_orient_matrix_UB_12      -0.0928375000
_diffrn_orient_matrix_UB_13      -0.0661179000
_diffrn_orient_matrix_UB_21      0.0889457000
_diffrn_orient_matrix_UB_22      -0.0338430000
_diffrn_orient_matrix_UB_23      0.0749912000
_diffrn_orient_matrix_UB_31      -0.1363578000
_diffrn_orient_matrix_UB_32      -0.0754857000
_diffrn_orient_matrix_UB_33      0.0105839000
_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  0.0342
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46922
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.609
_diffrn_reflns_theta_min         2.884
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.971
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.923
_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 blackish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0607P)^2^+1.8231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7807
_reflns_number_total             8305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd432
_cod_original_cell_volume        2052.99(6)
_cod_database_code               7711343
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P Fe'
_chemical_oxdiff_usercomment     'Ana sample'
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.721
_reflns_odcompleteness_completeness 99.97
_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
2.a Ternary CH refined with riding coordinates:
 C6(H6), C26(H26), C20(H20), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C9(H9A,H9B), C27(H27A,H27B), C11(H11A,H11B), C8(H8A,H8B), C7(H7A,
 H7B), C21(H21A,H21B), C28(H28A,H28B), C31(H31A,H31B), C10(H10A,H10B), C24(H24A,
 H24B), C19(H19A,H19B), C25(H25A,H25B), C17(H17A,H17B), C23(H23A,H23B),
 C29(H29A,H29B), C13(H13A,H13B), C30(H30A,H30B), C14(H14A,H14B), C22(H22A,H22B),
  C15(H15A,H15B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C33(H33), C38(H38), C39(H39), C37(H37), C40(H40), C46(H46),
 C44(H44), C34(H34), C45(H45), C41(H41), C3(H3), C2(H2), C35(H35), C36(H36)
;
_shelx_res_checksum              64655
_shelx_hkl_checksum              49478
_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 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.828