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

data_7711345
_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         'C52 H72 B Fe N O2 P2'
_chemical_formula_sum            'C52 H72 B Fe N O2 P2'
_chemical_formula_weight         871.70
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2021-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-02 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                106.5400(10)
_cell_angle_beta                 91.6510(10)
_cell_angle_gamma                95.6260(10)
_cell_formula_units_Z            1
_cell_length_a                   10.58760(10)
_cell_length_b                   10.63030(10)
_cell_length_c                   10.87050(10)
_cell_measurement_reflns_used    18521
_cell_measurement_temperature    99.97(15)
_cell_measurement_theta_max      76.3020
_cell_measurement_theta_min      4.1950
_cell_volume                     1165.13(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_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    -25.00  69.00   0.50    0.05    --   46.87 -74.00  -0.00  188
  2  \w     34.00  96.00   0.50    0.05    --   46.87-125.00 -30.00  124
  3  \w     34.00  93.00   0.50    0.18    --  106.69 -74.00  -0.00  118
  4  \w     34.00 106.00   0.50    0.18    --  106.69 -97.00 -93.14  144
  5  \w     34.00 111.00   0.50    0.18    --  106.69-125.00 -90.00  154
  6  \w     34.00 105.00   0.50    0.18    --  106.69 -94.00 -30.00  142
  7  \w     34.00 111.00   0.50    0.18    --  106.69-125.00  90.00  154
  8  \w     34.00 111.00   0.50    0.18    --  106.69-125.00 150.00  154
  9  \w     34.00  71.00   0.50    0.18    --  106.69 -61.00 150.00   74
 10  \w     34.00 105.00   0.50    0.18    --  106.69 -94.00 150.00  142
 11  \w     34.00  71.00   0.50    0.18    --  106.69 -61.00  60.00   74
 12  \w     34.00 109.00   0.50    0.18    --  106.69-118.00  63.92  150
 13  \w     34.00  71.00   0.50    0.18    --  106.69 -61.00 -90.00   74
 14  \w     34.00  71.00   0.50    0.18    --  106.69 -61.00 -60.00   74
 15  \w     34.00 105.00   0.50    0.18    --  106.69 -94.00-120.00  142
 16  \w     32.00 120.00   0.50    0.05    --   46.87  52.00  68.21  176
 17  \w     84.00 178.00   0.50    0.18    --  106.69  74.00 127.00  188
 18  \w     95.00 178.00   0.50    0.18    --  106.69 125.00 120.00  166
 19  \w     95.00 178.00   0.50    0.18    --  106.69 125.00 150.00  166
 20  \w    101.00 178.00   0.50    0.18    --  106.69  77.00-120.00  154
 21  \w     91.00 178.00   0.50    0.18    --  106.69  61.00-150.00  174
 22  \w     34.00 105.00   0.50    0.18    --  106.69 -94.00 120.00  142
 23  \w     32.00  80.00   0.50    0.05    --   46.87  51.00 -32.09   96
 24  \w     31.00 120.00   0.50    0.05    --   46.87  55.00-112.52  178
 25  \w     25.00 120.00   0.50    0.05    --   46.87  74.00 127.00  190
 26  \w    -30.00  29.00   0.50    0.05    --  -46.87  19.00 120.00  118
 27  \w    -51.00 -16.00   0.50    0.18    --  -88.50  45.00  90.00   70
 28  \w    -51.00 -16.00   0.50    0.18    --  -88.50  45.00 120.00   70
 29  \w    -69.00  26.00   0.50    0.05    --  -46.87  74.00 127.00  190
 30  \w    -51.00 -16.00   0.50    0.18    --  -88.50  45.00 -30.00   70
 31  \w    -51.00 -16.00   0.50    0.18    --  -88.50  45.00 -90.00   70
 32  \w    -51.00 -16.00   0.50    0.18    --  -88.50  45.00-150.00   70
 33  \w    -51.00 -16.00   0.50    0.18    --  -88.50  45.00 -60.00   70
 34  \w    -93.00 -15.00   0.50    0.18    --  -88.50  74.00 127.00  156
 35  \w   -120.00 -24.00   0.50    0.05    --  -46.87 -74.00  -0.00  192
 36  \w   -120.00 -88.00   0.50    0.05    --  -46.87-125.00 -30.00   64
 37  \w   -160.00 -66.00   0.50    0.18    --  -88.50 -74.00  -0.00  188
 38  \w   -160.00 -91.00   0.50    0.18    --  -88.50 -61.00 150.00  138
 39  \w   -160.00-100.00   0.50    0.18    --  -88.50 -94.00 150.00  120
 40  \w   -160.00-101.00   0.50    0.18    --  -88.50 -77.00  60.00  118
 41  \w   -160.00-101.00   0.50    0.18    --  -88.50 -77.00 120.00  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      -0.0531062000
_diffrn_orient_matrix_UB_12      0.0449507000
_diffrn_orient_matrix_UB_13      0.1341188000
_diffrn_orient_matrix_UB_21      -0.1079884000
_diffrn_orient_matrix_UB_22      -0.1143343000
_diffrn_orient_matrix_UB_23      -0.0413276000
_diffrn_orient_matrix_UB_31      0.0834950000
_diffrn_orient_matrix_UB_32      -0.0896998000
_diffrn_orient_matrix_UB_33      0.0473010000
_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  0.0376
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22425
_diffrn_reflns_point_group_measured_fraction_full 0.806
_diffrn_reflns_point_group_measured_fraction_max 0.753
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.568
_diffrn_reflns_theta_min         4.203
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.545
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.559
_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 reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       plate
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.007(3)
_refine_ls_extinction_coef       0.0011(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7375
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0573P)^2^+0.2321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.554
_reflns_Friedel_fraction_full    0.613
_reflns_Friedel_fraction_max     0.537
_reflns_number_gt                7228
_reflns_number_total             7375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd433
_cod_database_code               7711345
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P B'
_chemical_oxdiff_usercomment     'Ana borane sample'
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.520
_reflns_odcompleteness_completeness 99.95
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6), C19(H19), C12(H12), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C15(H15A,H15B), C18(H18A,H18B), C26(H26A,
 H26B), C24(H24A,H24B), C28(H28A,H28B), C20(H20A,H20B), C11(H11A,H11B),
 C21(H21A,H21B), C13(H13A,H13B), C27(H27A,H27B), C23(H23A,H23B), C7(H7A,H7B),
 C14(H14A,H14B), C10(H10A,H10B), C29(H29A,H29B), C5(H5A,H5B), C30(H30A,H30B),
 C22(H22A,H22B), C8(H8A,H8B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C42(H42), C44(H44), C46(H46), C45(H45), C40(H40), C2(H2), C38(H38),
 C3(H3), C36(H36), C37(H37), C39(H39)
2.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C49(H49A,H49B,
 H49C)
;
_shelx_res_checksum              88777
_shelx_hkl_checksum              97331
_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 1.442
_oxdiff_exptl_absorpt_empirical_full_min 0.706