A reagent for heteroatom borylation, including iron mediated reductive deoxygenation of nitrate yielding a dinitrosyl complex.
Beagan, Daniel M.; Carta, Veronica; Caulton, Kenneth G.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1681–1687; doi:10.1039/d0dt00077a

data_7703324
_publ_section_title
;
 A reagent for heteroatom borylation, including iron mediated reductive
 deoxygenation of nitrate yielding a dinitrosyl complex.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1681
_journal_page_last               1687
_journal_paper_doi               10.1039/d0dt00077a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C24 H31 Fe N5 O6, 2(C2 H3 N)'
_chemical_formula_sum            'C28 H37 Fe N7 O6'
_chemical_formula_weight         623.49
_chemical_name_systematic        (DIM)Fe(NO3)2(MeCN)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-03 deposited with the CCDC.	2020-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0228(4)
_cell_length_b                   11.6142(4)
_cell_length_c                   15.9579(5)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.48
_cell_volume                     3154.98(16)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38729
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.078
_diffrn_reflns_theta_max         25.078
_diffrn_reflns_theta_min         2.123
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex3 (Bruker, 2016)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_preparation       synthesized
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 2255 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5587
_refine_ls_number_restraints     349
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                5084
_reflns_number_total             5587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00077a2.cif
_cod_data_source_block           19088_0ma
_cod_depositor_comments
'Adding full bibliography for 7703323--7703325.cif.'
_cod_database_code               7703324
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.809
_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. Rigid bond restraints
 Fe1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Fe1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Fe1, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O1 \\sim Fe1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O4 \\sim Fe1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C20(H20), C17(H17), C3(H3)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C22(H22A,H22B,
 H22C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C1(H1A,H1B,H1C), C26(H26A,
 H26B,H26C), C19(H19A,H19B,H19C), C5(H5A,H5B,H5C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              96609
_olex2_date_sample_data_collection 2019-06-29
_olex2_date_sample_submission    2019-05-26
_olex2_submission_original_sample_id dmb_23
_olex2_submission_special_instructions 'No special instructions were received'