Olefin hydroboration catalyzed by an iron-borane complex.
Grose, Laura A.; Willcox, Darren; Chemical communications (Cambridge, England) 59 (2023) 7427–7430; doi:10.1039/d3cc00494e

data_7131700
_publ_section_title
;
 Olefin hydroboration catalyzed by an iron-borane complex.
;
_journal_issue                   48
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7427
_journal_page_last               7430
_journal_paper_doi               10.1039/d3cc00494e
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C30 H52 B2 Fe O2 P2'
_chemical_formula_sum            'C30 H52 B2 Fe O2 P2'
_chemical_formula_weight         584.12
_chemical_name_systematic        '[(eta3-H2iprDPB)Fe(eta3-H2Bpin)]'
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-02 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.869(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6026(3)
_cell_length_b                   10.9986(3)
_cell_length_c                   29.9514(8)
_cell_measurement_reflns_used    10148
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      28.9080
_cell_measurement_theta_min      2.8120
_cell_volume                     3151.91(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.887
_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    -92.00   0.00   1.00    2.80    --  -18.77 -19.00 120.00   92
  2  \w    -39.00   3.00   1.00    2.80    --  -18.77 -77.00 -90.00   42
  3  \w      7.00  35.00   1.00    2.80    --   20.49  77.00-150.00   28
  4  \w     -9.00  40.00   1.00    2.80    --   20.49  77.00 150.00   49
  5  \w     49.00  98.00   1.00    2.80    --   20.49 178.00  90.00   49
  6  \w    -16.00  95.00   1.00    2.80    --   20.49  19.00  30.00  111
  7  \w     -6.00  20.00   1.00    2.80    --   20.49  37.00 120.00   26
  8  \w     57.00  98.00   1.00    2.80    --   20.49 178.00 -60.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0227353000
_diffrn_orient_matrix_UB_12      0.0582751000
_diffrn_orient_matrix_UB_13      0.0064122000
_diffrn_orient_matrix_UB_21      0.0588934000
_diffrn_orient_matrix_UB_22      0.0268176000
_diffrn_orient_matrix_UB_23      -0.0088609000
_diffrn_orient_matrix_UB_31      -0.0388014000
_diffrn_orient_matrix_UB_32      0.0064770000
_diffrn_orient_matrix_UB_33      -0.0211217000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26248
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.132
_diffrn_reflns_theta_min         2.290
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (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 reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method
'slow evaporation from diethyl ether at room temperature'
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0271P)^2^+1.4312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6241
_reflns_number_total             7510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00494e2.cif
_cod_data_source_block           adw_13
_cod_depositor_comments          'Adding full bibliography for 7131700.cif.'
_cod_original_cell_volume        3151.93(16)
_cod_database_code               7131700
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe B P2 H C'
_chemical_oxdiff_usercomment     pink
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C20(H20), C26(H26), C14(H14)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C4(H4), C7(H7), C18(H18), C1(H1), C2(H2), C9AA(H9AA), C9(H9)
2.c Idealised Me refined as rotating group:
 C0AA(H0Aa,H0Ab,H0Ac), C23(H23a,H23b,H23c), C27(H27a,H27b,H27c), C6(H6a,H6b,
 H6c), C10(H10a,H10b,H10c), C8AA(H8Aa,H8Ab,H8Ac), C3AA(H3Aa,H3Ab,H3Ac),
 C6AA(H6Aa,H6Ab,H6Ac), C7AA(H7Aa,H7Ab,H7Ac), C5AA(H5Aa,H5Ab,H5Ac), C4AA(H4Aa,
 H4Ab,H4Ac), C12(H12a,H12b,H12c)
;
_shelx_res_checksum              97005
_shelx_hkl_checksum              19972
_olex2_date_sample_data_collection 2023-04-21
_olex2_exptl_crystal_mounting_method 'fomblin oil'
_olex2_submission_original_sample_id adw13
_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.724