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

data_7711344
_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         'C88 H136 B2 Fe2 N2 O4 P4, C7 H15'
_chemical_formula_sum            'C95 H151 B2 Fe2 N2 O4 P4'
_chemical_formula_weight         1642.37
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-21
_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                 106.741(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7870(3)
_cell_length_b                   23.7592(7)
_cell_length_c                   17.1342(4)
_cell_measurement_reflns_used    13557
_cell_measurement_temperature    99.99(11)
_cell_measurement_theta_max      74.8580
_cell_measurement_theta_min      2.7730
_cell_volume                     4595.1(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-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      99.99(11)
_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    -81.00   1.00   0.50   18.90    --  -46.37 107.00  72.00  164
  2  \w    -51.00 -16.00   0.50   75.90    --  -88.50  45.00  30.00   70
  3  \w    -81.00 -15.00   0.50   75.90    --  -88.50 107.00  72.00  132
  4  \w    -45.00 -19.00   0.50   75.90    --  -88.50  45.00-120.00   52
  5  \w    -51.00 -26.00   0.50   75.90    --  -88.50  45.00-150.00   50
  6  \w   -118.00 -83.00   0.50   18.90    --  -46.37 -57.00  30.00   70
  7  \w   -118.00 -83.00   0.50   18.90    --  -46.37 -57.00 120.00   70
  8  \w   -118.00 -83.00   0.50   18.90    --  -46.37 -57.00 150.00   70
  9  \w   -160.00 -91.00   0.50   75.90    --  -88.50 -61.00  90.00  138
 10  \w   -160.00 -83.00   0.50   75.90    --  -88.50-107.00 -25.00  154
 11  \w   -118.00 -83.00   0.50   18.90    --  -46.37 -57.00 -90.00   70
 12  \w   -118.00 -87.00   0.50   18.90    --  -46.37-125.00-150.00   62
 13  \w   -118.00 -87.00   0.50   18.90    --  -46.37-125.00-180.00   62
 14  \w   -118.00 -87.00   0.50   18.90    --  -46.37-125.00-120.00   62
 15  \w   -142.00-116.00   0.50   75.90    --  -88.50 -77.00-150.00   52
 16  \w     20.00  85.00   0.50   18.90    --   46.37-107.00 -25.00  130
 17  \w     34.00 108.00   0.50   75.90    --  106.69-107.00 -25.00  148
 18  \w     81.00 107.00   0.50   75.90    --  106.69-125.00  60.00   52
 19  \w     39.00  71.00   0.50   75.90    --  106.69 -61.00 150.00   64
 20  \w     44.00  70.00   0.50   75.90    --  106.69 -61.00 120.00   52
 21  \w     34.00  71.00   0.50   75.90    --  106.69 -61.00  30.00   74
 22  \w     43.00 101.00   0.50   75.90    --  106.69 -77.00  30.00  116
 23  \w     53.00  91.00   0.50   75.90    --  106.69 -77.00 -90.00   76
 24  \w     34.00  59.00   0.50   75.90    --  106.69 -61.00-180.00   50
 25  \w     42.00  71.00   0.50   75.90    --  106.69 -61.00-120.00   58
 26  \w     36.00  82.00   0.50   75.90    --  106.69 -77.00 -30.00   92
 27  \w     37.00  69.00   0.50   75.90    --  106.69-125.00  60.00   64
 28  \w     83.00 118.00   0.50   18.90    --   46.37  57.00 -90.00   70
 29  \w    105.00 178.00   0.50   75.90    --  106.69 107.00  72.00  146
 30  \w     83.00 118.00   0.50   18.90    --   46.37  57.00 150.00   70
 31  \w     83.00 118.00   0.50   18.90    --   46.37  57.00  60.00   70
 32  \w     91.00 172.00   0.50   75.90    --  106.69  61.00 120.00  162
 33  \w     93.00 174.00   0.50   75.90    --  106.69  45.00 150.00  162
;
_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      0.0421553000
_diffrn_orient_matrix_UB_12      0.0578827000
_diffrn_orient_matrix_UB_13      0.0377191000
_diffrn_orient_matrix_UB_21      -0.1231703000
_diffrn_orient_matrix_UB_22      0.0249268000
_diffrn_orient_matrix_UB_23      -0.0421735000
_diffrn_orient_matrix_UB_31      -0.0410837000
_diffrn_orient_matrix_UB_32      -0.0151827000
_diffrn_orient_matrix_UB_33      0.0749657000
_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  0.0757
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            42860
_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         70.000
_diffrn_reflns_theta_min         3.273
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.561
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.912
_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    1.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             1778
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+12.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6978
_reflns_number_total             8663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02879d2.cif
_cod_data_source_block           hpd066a
_cod_original_cell_volume        4595.0(2)
_cod_database_code               7711344
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Fe1B1N2P2C20h20
_chemical_oxdiff_usercomment     'Ana sample'
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.776
_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. Others
 Fixed Sof: C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5)
3.a Ternary CH refined with riding coordinates:
 C15(H15), C23(H23), C2(H2), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C20(H20A,H20B), C9(H9A,H9B), C19(H19A,H19B), C21(H21A,H21B),
 C18(H18A,H18B), C27(H27A,H27B), C3(H3A,H3B), C26(H26A,H26B), C17(H17A,H17B),
 C24(H24A,H24B), C25(H25A,H25B), C16(H16A,H16B), C7(H7A,H7B), C5(H5A,H5B),
 C6(H6A,H6B), C34(H34A,H34B), C4(H4A,H4B), C33(H33A,H33B), C30(H30A,H30B),
 C32(H32A,H32B), C31(H31A,H31B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
3.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C40(H40), C39(H39), C13(H13), C37(H37), C42(H42), C38(H38), C12(H12)
3.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C48(H48A,H48B,
 H48C), C55(H55A,H55B,H55C)
;
_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 2.205
_oxdiff_exptl_absorpt_empirical_full_min 0.478