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

data_7711341
_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         'C17 H14 B N O3'
_chemical_formula_sum            'C17 H14 B N O3'
_chemical_formula_weight         291.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-02 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4635(2)
_cell_length_b                   16.0928(3)
_cell_length_c                   7.7560(2)
_cell_measurement_reflns_used    5603
_cell_measurement_temperature    100.01(14)
_cell_measurement_theta_max      75.0460
_cell_measurement_theta_min      4.7350
_cell_volume                     1430.83(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      100.01(14)
_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 0.959
_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    -40.00  28.00   0.50   22.00    --  -46.75  33.00 145.00  136
  2  \w    -51.00 -16.00   0.50   88.00    --  -88.50  45.00 120.00   70
  3  \w    -80.00 -15.00   0.50   88.00    --  -88.50  89.00 -45.00  130
  4  \w    -43.00  27.00   0.50   22.00    --  -46.75  37.00-150.00  140
  5  \w    -51.00 -16.00   0.50   88.00    --  -88.50  45.00-180.00   70
  6  \w   -119.00 -83.00   0.50   22.00    --  -46.75 -57.00   0.00   72
  7  \w   -119.00 -83.00   0.50   22.00    --  -46.75 -57.00  60.00   72
  8  \w   -121.00 -32.00   0.50   22.00    --  -46.75 -37.00  60.00  178
  9  \w   -119.00 -88.00   0.50   22.00    --  -46.75-125.00 150.00   62
 10  \w   -163.00 -74.00   0.50   88.00    --  -88.50 -33.00 -13.00  178
 11  \w   -121.00 -32.00   0.50   22.00    --  -46.75 -37.00-150.00  178
 12  \w   -119.00 -83.00   0.50   22.00    --  -46.75 -57.00-180.00   72
 13  \w   -160.00 -91.00   0.50   88.00    --  -88.50 -61.00-150.00  138
 14  \w   -161.00 -82.00   0.50   88.00    --  -88.50 -45.00  90.00  158
 15  \w     34.00 111.00   0.50   88.00    --  106.69-125.00 125.00  154
 16  \w     34.00  71.00   0.50   88.00    --  106.69 -61.00  90.00   74
 17  \w     34.00  71.00   0.50   88.00    --  106.69 -61.00   0.00   74
 18  \w     34.00  71.00   0.50   88.00    --  106.69 -61.00 -90.00   74
 19  \w     34.00  71.00   0.50   88.00    --  106.69 -61.00-120.00   74
 20  \w     34.00 101.00   0.50   88.00    --  106.69 -77.00-180.00  134
;
_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      -0.0273239000
_diffrn_orient_matrix_UB_12      -0.0337687000
_diffrn_orient_matrix_UB_13      -0.0923124000
_diffrn_orient_matrix_UB_21      -0.1191557000
_diffrn_orient_matrix_UB_22      -0.0769287000
_diffrn_orient_matrix_UB_23      0.0244414000
_diffrn_orient_matrix_UB_31      -0.0558843000
_diffrn_orient_matrix_UB_32      0.1799124000
_diffrn_orient_matrix_UB_33      -0.0069064000
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10603
_diffrn_reflns_point_group_measured_fraction_full 0.870
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.113
_diffrn_reflns_theta_min         4.736
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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 grayish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.135
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2419
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0376P)^2^+0.2682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.561
_reflns_Friedel_fraction_full    0.717
_reflns_Friedel_fraction_max     0.627
_reflns_number_gt                2273
_reflns_number_total             2419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd501b
_cod_database_code               7711341
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe N P C H O B'
_chemical_oxdiff_usercomment     'Catalytic borane sample'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C3(H3), C16(H16), C2(H2), C5(H5), C8(H8), C10(H10),
 C4(H4), C9(H9), C17(H17), C11(H11), C14(H14), C15(H15)
;
_shelx_res_checksum              75844
_shelx_hkl_checksum              2861
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.745