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

data_7711342
_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         'C38 H55 Fe N O3 P2'
_chemical_formula_sum            'C38 H55 Fe N O3 P2'
_chemical_formula_weight         691.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-09
_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                 98.5190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.61150(10)
_cell_length_b                   14.9766(2)
_cell_length_c                   17.44500(10)
_cell_measurement_reflns_used    20374
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3070
_cell_measurement_theta_min      3.2790
_cell_volume                     3517.00(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)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.993
_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     83.00 120.00   0.50    1.15    --   46.87  57.00-150.00   74
  2  \w     83.00 120.00   0.50    1.15    --   46.87  57.00-180.00   74
  3  \w    141.00 178.00   0.50    4.60    --  106.69  61.00 -30.00   74
  4  \w     91.00 178.00   0.50    4.60    --  106.69 131.00  -2.00  174
  5  \w     87.00 178.00   0.50    4.60    --  106.69 137.00 173.00  182
  6  \w     92.00 178.00   0.50    4.60    --  106.69  45.00  90.00  172
  7  \w     94.00 124.00   0.50    4.60    --  106.69  61.00 -30.00   60
  8  \w     37.00  62.00   0.50    4.60    --  106.69 -61.00  90.00   50
  9  \w     74.00 107.00   0.50    4.60    --  106.69-104.00  94.25   66
 10  \w     41.00 102.00   0.50    1.15    --   46.87-137.00 111.00  122
 11  \w     41.00 120.00   0.50    4.60    --  106.69-137.00 111.00  158
 12  \w     38.00  99.00   0.50    1.15    --   46.87-131.00 -72.00  122
 13  \w     38.00 116.00   0.50    4.60    --  106.69-131.00 -72.00  156
 14  \w     72.00 106.00   0.50    4.60    --  106.69-102.00 -62.47   68
 15  \w     34.00  92.00   0.50    4.60    --  106.69 -77.00 -60.00  116
 16  \w     35.00  71.00   0.50    4.60    --  106.69 -61.00   0.00   72
 17  \w     34.00  90.00   0.50    4.60    --  106.69 -94.00 -60.00  112
 18  \w    -91.00 -16.00   0.50    1.15    --  -46.87 131.00  -2.00  150
 19  \w    -51.00 -16.00   0.50    4.60    --  -88.50  45.00 150.00   70
 20  \w    -51.00 -16.00   0.50    4.60    --  -88.50  45.00 120.00   70
 21  \w    -95.00 -19.00   0.50    1.15    --  -46.87 137.00 173.00  152
 22  \w    -95.00 -19.00   0.50    4.60    --  -88.50 137.00 173.00  152
 23  \w   -120.00 -83.00   0.50    1.15    --  -46.87 -57.00 150.00   74
 24  \w   -120.00 -83.00   0.50    1.15    --  -46.87 -57.00 120.00   74
 25  \w   -120.00 -66.00   0.50    1.15    --  -46.87-137.00 111.00  108
 26  \w   -120.00 -70.00   0.50    1.15    --  -46.87-131.00 -72.00  100
 27  \w   -120.00 -83.00   0.50    1.15    --  -46.87 -57.00-180.00   74
 28  \w   -160.00 -70.00   0.50    4.60    --  -88.50-131.00 -72.00  180
 29  \w   -160.00-101.00   0.50    4.60    --  -88.50 -77.00-120.00  118
 30  \w    -51.00 -16.00   0.50    4.60    --  -88.50  45.00-180.00   70
 31  \w    -51.00 -16.00   0.50    4.60    --  -88.50  45.00-120.00   70
 32  \w    -51.00 -16.00   0.50    4.60    --  -88.50  45.00-150.00   70
;
_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      -0.0042214000
_diffrn_orient_matrix_UB_12      -0.0815169000
_diffrn_orient_matrix_UB_13      -0.0543153000
_diffrn_orient_matrix_UB_21      -0.0099033000
_diffrn_orient_matrix_UB_22      0.0627122000
_diffrn_orient_matrix_UB_23      -0.0707164000
_diffrn_orient_matrix_UB_31      0.1139012000
_diffrn_orient_matrix_UB_32      0.0023822000
_diffrn_orient_matrix_UB_33      0.0051707000
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39701
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.984
_diffrn_reflns_theta_min         3.909
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.583
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.807
_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 dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.062
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0400P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6200
_reflns_number_total             6614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd065
_cod_database_code               7711342
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Fe1O1P2N2C20H20
_chemical_oxdiff_usercomment     'Ana Sample orange crystal'
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.618
_reflns_odcompleteness_completeness 99.92
_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:
 C19(H19), C6(H6), C12(H12), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C26(H26A,H26B), C27(H27A,H27B), C5(H5A,H5B),
 C24(H24A,H24B), C29(H29A,H29B), C17(H17A,H17B), C7(H7A,H7B), C18(H18A,H18B),
 C11(H11A,H11B), C8(H8A,H8B), C23(H23A,H23B), C21(H21A,H21B), C28(H28A,H28B),
 C14(H14A,H14B), C30(H30A,H30B), C22(H22A,H22B), C15(H15A,H15B), C16(H16A,H16B),
  C10(H10A,H10B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C36(H36), C32(H32), C34(H34), C33(H33), C35(H35)
;
_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 1.484
_oxdiff_exptl_absorpt_empirical_full_min 0.639