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

data_7711346
_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         'C40 H60 B Fe N O2 P2'
_chemical_formula_sum            'C40 H60 B Fe N O2 P2'
_chemical_formula_weight         715.49
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-10-31
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2022-09-02 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.77930(10)
_cell_length_b                   19.2148(2)
_cell_length_c                   18.68470(10)
_cell_measurement_reflns_used    25949
_cell_measurement_temperature    100.02(18)
_cell_measurement_theta_max      76.2560
_cell_measurement_theta_min      2.3220
_cell_volume                     3773.35(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 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_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    -74.00  26.00   0.50    0.75    --  -46.87  84.00-144.00  200
  2  \w    -21.00  74.00   0.50    0.75    --   46.87 -84.00  95.00  190
  3  \w   -109.00 -15.00   0.50    2.02    --  -88.50  84.00-144.00  188
  4  \w     34.00 121.00   0.50    2.02    --  106.69 -84.00  95.00  174
  5  \w    101.00 178.00   0.50    2.02    --  106.69  84.00-144.00  154
  6  \w   -120.00 -83.00   0.50    0.75    --  -46.87 -57.00 -60.00   74
  7  \w   -120.00 -87.00   0.50    0.75    --  -46.87-125.00 -90.00   66
  8  \w   -120.00 -83.00   0.50    0.75    --  -46.87 -57.00 120.00   74
  9  \w   -120.00 -87.00   0.50    0.75    --  -46.87-125.00 -30.00   66
 10  \w   -120.00 -87.00   0.50    0.75    --  -46.87-125.00-180.00   66
 11  \w     83.00 120.00   0.50    0.75    --   46.87  57.00-150.00   74
 12  \w    -47.00 -16.00   0.50    2.02    --  -88.50  45.00-150.00   62
 13  \w    -38.00 -12.00   0.50    2.02    --  -88.50  15.00  30.00   52
 14  \w    -64.00 -15.00   0.50    2.02    --  -88.50  61.00-150.00   98
 15  \w    -47.00 -16.00   0.50    2.02    --  -88.50  45.00-180.00   62
 16  \w   -160.00-101.00   0.50    2.02    --  -88.50 -77.00-180.00  118
 17  \w    -38.00 -12.00   0.50    2.02    --  -88.50  15.00  60.00   52
 18  \w    -47.00 -16.00   0.50    2.02    --  -88.50  45.00  60.00   62
 19  \w   -160.00 -79.00   0.50    2.02    --  -88.50 -84.00  95.00  162
 20  \w    101.00 178.00   0.50    2.02    --  106.69  77.00 -30.00  154
 21  \w    101.00 178.00   0.50    2.02    --  106.69  77.00  90.00  154
 22  \w     34.00 100.00   0.50    2.02    --  106.69 -77.00   0.00  132
 23  \w     34.00  76.00   0.50    2.02    --  106.69 -61.00 120.00   84
 24  \w     34.00 111.00   0.50    2.02    --  106.69-125.00  90.00  154
 25  \w     34.00  76.00   0.50    2.02    --  106.69 -61.00-120.00   84
 26  \w     91.00 178.00   0.50    2.02    --  106.69  30.00 120.00  174
 27  \w     34.00  76.00   0.50    2.02    --  106.69 -61.00-180.00   84
 28  \w     34.00  76.00   0.50    2.02    --  106.69 -61.00 150.00   84
 29  \w   -121.00 -94.00   0.50    0.75    --  -46.87 -37.00-180.00   54
 30  \w   -121.00 -32.00   0.50    0.75    --  -46.87 -37.00 -30.00  178
;
_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      -0.0281824000
_diffrn_orient_matrix_UB_12      -0.0641766000
_diffrn_orient_matrix_UB_13      0.0432682000
_diffrn_orient_matrix_UB_21      -0.1333328000
_diffrn_orient_matrix_UB_22      0.0290844000
_diffrn_orient_matrix_UB_23      -0.0003533000
_diffrn_orient_matrix_UB_31      -0.0540540000
_diffrn_orient_matrix_UB_32      -0.0382424000
_diffrn_orient_matrix_UB_33      -0.0726465000
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43766
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.488
_diffrn_reflns_theta_min         3.343
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.263
_exptl_absorpt_correction_T_max  0.65024
_exptl_absorpt_correction_T_min  0.62475
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.055
_exptl_crystal_size_rad          0.0385
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0402P)^2^+3.1653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7239
_reflns_number_total             7662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd021
_cod_database_code               7711346
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Fe1B1P2N2O2C20H20
_chemical_oxdiff_usercomment     'Ana Alkyne 2'
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.616
_reflns_odcompleteness_completeness 100.00
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H13C(0.6) H13D(0.6) H13A(0.4) H13B(0.4) H16A(0.6) H16B(0.6)
 H16C(0.4) H16D(0.4) H12(0.6) H12A(0.4) C17B(0.6) H17A(0.6) H17B(0.6) C17A(0.4)
 H17C(0.4) H17D(0.4) C15B(0.6) H15A(0.6) H15B(0.6) C15A(0.4) H15C(0.4)
 H15D(0.4) C14B(0.6) H14A(0.6) H14B(0.6) C14A(0.4) H14C(0.4) H14D(0.4)
3.a Ternary CH refined with riding coordinates:
 C19(H19), C6(H6), C25(H25), C12(H12), C12(H12A)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C18(H18A,H18B), C24(H24A,H24B), C8(H8A,H8B), C11(H11A,H11B),
 C26(H26A,H26B), C5(H5A,H5B), C20(H20A,H20B), C27(H27A,H27B), C23(H23A,H23B),
 C29(H29A,H29B), C28(H28A,H28B), C30(H30A,H30B), C13(H13C,H13D), C13(H13A,H13B),
  C9(H9A,H9B), C22(H22A,H22B), C10(H10A,H10B), C21(H21A,H21B), C16(H16A,H16B),
 C16(H16C,H16D), C17B(H17A,H17B), C17A(H17C,H17D), C15B(H15A,H15B), C15A(H15C,
 H15D), C14B(H14A,H14B), C14A(H14C,H14D)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C35(H35), C32(H32), C34(H34), C33(H33)
3.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              1958
_shelx_hkl_checksum              46377
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.356
_oxdiff_exptl_absorpt_empirical_full_min 0.752