Electrophile-promoted Fe-to-N<sub>2</sub> hydride migration in highly reduced Fe(N<sub>2</sub>)(H) complexes.
Deegan, Meaghan M.; Peters, Jonas C.; Chemical science 9 (2018) 6264–6270; doi:10.1039/c8sc02380h

data_1549629
_publ_section_title
;
 Electrophile-promoted Fe-to-N<sub>2</sub> hydride migration in highly
 reduced Fe(N<sub>2</sub>)(H) complexes.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              6264
_journal_page_last               6270
_journal_paper_doi               10.1039/c8sc02380h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C48 H86 B Fe K2 N2 O6 P3'
_chemical_formula_sum            'C48 H86 B Fe K2 N2 O6 P3'
_chemical_formula_weight         1024.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-30 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.668(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8973(7)
_cell_length_b                   12.5342(6)
_cell_length_c                   17.2106(8)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.7461
_cell_measurement_theta_min      0.6655
_cell_volume                     2750.4(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.04
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            76519
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         2.459
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0838 before and 0.0599 after correction. The Ratio of minimum to maximum transmission is 0.8920. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       blob
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 5215 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         14778
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0370P)^2^+0.3220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.758
_reflns_number_gt                13242
_reflns_number_total             14778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02380h2.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
'Adding full bibliography for 1549629--1549633.cif.'
_cod_database_code               1549629
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.887
_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. Uiso/Uaniso restraints and constraints
C18B \\sim C16B \\sim C16A \\sim C17B \\sim C17A \\sim C18A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C18B, C16B, C16A, C18A, C17B, C17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C16B)=Sof(H16B)=Sof(C17B)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C1(H1), C13(H13), C25(H25), C28(H28), C16A(H16A), C16B(H16B)
5.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C38(H38A,H38B), C46(H46A,H46B), C43(H43A,H43B), C47(H47A,H47B)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C21(H21), C9(H9), C35(H35), C20(H20), C11(H11), C22(H22),
 C34(H34), C23(H23), C32(H32), C33(H33)
5.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C15(H15A,H15B,H15C),
 C2(H2A,H2B,H2C), C27(H27A,H27B,H27C), C14(H14A,H14B,H14C), C6(H6A,H6B,H6C),
 C30(H30A,H30B,H30C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C29(H29A,H29B,
 H29C), C45(H45A,H45B,H45C), C17A(H17A,H17B,H17C), C44(H44A,H44B,H44C),
 C48(H48A,H48B,H48C), C37(H37A,H37B,H37C), C18A(H18A,H18B,H18C), C18B(H18D,H18E,
 H18F), C17B(H17D,H17E,H17F)
;
_shelx_res_checksum              56807
_olex2_submission_special_instructions 'No special instructions were received'