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

data_7711347
_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_absolute_configuration ad
_chemical_formula_moiety         'C44 H60 B Fe N O2 P2'
_chemical_formula_sum            'C44 H60 B Fe N O2 P2'
_chemical_formula_weight         763.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 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                 102.5890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.72790(10)
_cell_length_b                   10.37420(10)
_cell_length_c                   20.4740(2)
_cell_measurement_reflns_used    19340
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.7090
_cell_measurement_theta_min      4.2400
_cell_volume                     2016.54(4)
_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      100.01(10)
_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 0.958
_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    -65.00  26.00   0.50    0.20    --  -46.87  64.00 -24.00  182
  2  \w   -120.00 -28.00   0.50    0.20    --  -46.87 -64.00-160.00  184
  3  \w     29.00 120.00   0.50    0.20    --   46.87  64.00 -24.00  182
  4  \w    -25.00  65.00   0.50    0.20    --   46.87 -64.00-160.00  180
  5  \w   -160.00 -70.00   0.50    0.84    --  -88.50 -64.00-160.00  180
  6  \w    -67.00 -15.00   0.50    0.84    --  -88.50  64.00 -24.00  104
  7  \w     88.00 178.00   0.50    0.84    --  106.69  64.00 -24.00  180
  8  \w     34.00  80.00   0.50    0.84    --  106.69 -64.00-160.00   92
  9  \w   -120.00 -87.00   0.50    0.20    --  -46.87-125.00  30.00   66
 10  \w   -120.00 -87.00   0.50    0.20    --  -46.87-125.00   0.00   66
 11  \w    -86.00 -15.00   0.50    0.84    --  -88.50 125.00   0.00  142
 12  \w   -160.00-100.00   0.50    0.84    --  -88.50 -94.00 120.00  120
 13  \w    -38.00 -12.00   0.50    0.84    --  -88.50  15.00   0.00   52
 14  \w    -38.00 -12.00   0.50    0.84    --  -88.50  15.00 120.00   52
 15  \w    -38.00 -12.00   0.50    0.84    --  -88.50  15.00  60.00   52
 16  \w    -47.00 -16.00   0.50    0.84    --  -88.50  45.00 120.00   62
 17  \w    -38.00 -12.00   0.50    0.84    --  -88.50  15.00 -30.00   52
 18  \w     34.00  76.00   0.50    0.84    --  106.69 -61.00-120.00   84
 19  \w     34.00  76.00   0.50    0.84    --  106.69 -61.00 -30.00   84
 20  \w     89.00 178.00   0.50    0.84    --  106.69  15.00 -90.00  178
 21  \w     34.00 105.00   0.50    0.84    --  106.69 -94.00 120.00  142
 22  \w     34.00  76.00   0.50    0.84    --  106.69 -61.00 -90.00   84
 23  \w     34.00  76.00   0.50    0.84    --  106.69 -61.00 120.00   84
 24  \w     34.00  76.00   0.50    0.84    --  106.69 -61.00  90.00   84
 25  \w     32.00 121.00   0.50    0.20    --   46.87  37.00-180.00  178
 26  \w     32.00 121.00   0.50    0.20    --   46.87  37.00 -90.00  178
 27  \w     32.00 121.00   0.50    0.20    --   46.87  37.00 -30.00  178
 28  \w     32.00  75.00   0.50    0.20    --   46.87  37.00 120.00   86
 29  \w     32.00 121.00   0.50    0.20    --   46.87  37.00  90.00  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      0.1462702000
_diffrn_orient_matrix_UB_12      -0.0042350000
_diffrn_orient_matrix_UB_13      0.0476919000
_diffrn_orient_matrix_UB_21      -0.0499159000
_diffrn_orient_matrix_UB_22      -0.1108260000
_diffrn_orient_matrix_UB_23      0.0392922000
_diffrn_orient_matrix_UB_31      0.0496084000
_diffrn_orient_matrix_UB_32      -0.0987068000
_diffrn_orient_matrix_UB_33      -0.0460914000
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23310
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.489
_diffrn_reflns_theta_min         4.262
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.024
_exptl_absorpt_correction_T_max  0.57257
_exptl_absorpt_correction_T_min  0.53529
_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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.044
_exptl_crystal_size_rad          0.0552
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 3002 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7200
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0426P)^2^+0.4223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.852
_reflns_Friedel_fraction_max     0.749
_reflns_number_gt                7089
_reflns_number_total             7200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd_020
_cod_database_code               7711347
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Fe1N2P2O2B1C20H10
_chemical_oxdiff_usercomment     'Ana Alkyne'
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.503
_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), C25(H25), C19(H19), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C24(H24A,H24B), C26(H26A,H26B), C30(H30A,H30B), C23(H23A,
 H23B), C8(H8A,H8B), C9(H9A,H9B), C18(H18A,H18B), C27(H27A,H27B), C5(H5A,H5B),
 C7(H7A,H7B), C29(H29A,H29B), C17(H17A,H17B), C10(H10A,H10B), C13(H13A,H13B),
 C22(H22A,H22B), C20(H20A,H20B), C28(H28A,H28B), C21(H21A,H21B), C16(H16A,H16B),
  C14(H14A,H14B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C3(H3), C40(H40), C41(H41), C42(H42), C43(H43), C32(H32), C2(H2),
 C34(H34), C44(H44), C35(H35), C33(H33)
;
_shelx_res_checksum              30768
_shelx_hkl_checksum              33154
_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.818