Anion control of tautomeric equilibria: Fe‒H vs. N‒H influenced by NH⋯F hydrogen bonding
Chambers, Geoffrey M.; Johnson, Samantha I.; Raugei, Simone; Bullock, R. Morris; Chemical Science  (2019) –; doi:10.1039/C8SC04239J

data_1550282
_publ_section_title
;
 Anion control of tautomeric equilibria: Fe--H vs. N--H influenced by
 NH&#x22EF;F hydrogen bonding
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04239J
_journal_year                    2019
_chemical_formula_moiety         'C14 H29 Fe N O3 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C16 H29 F6 Fe N O9 P2 S2'
_chemical_formula_weight         675.31
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-14
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) 
;
_audit_update_record
;
2018-06-14 deposited with the CCDC.
2018-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.408(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.081(2)
_cell_length_b                   11.2301(14)
_cell_length_c                   15.4862(19)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.028
_cell_measurement_theta_min      2.273
_cell_volume                     2682.8(6)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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_radiation_wavelength_id  a89a_0m
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            93868
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.243
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.7426
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       Block
_exptl_crystal_F_000             1384
_exptl_crystal_id                a89a_0m
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research). 
;
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.218
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         8176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+3.0753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7331
_reflns_number_total             8176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04239j6.cif
_cod_data_source_block           a89a_0m_65
_cod_database_code               1550282
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.5 times of: 
  All C(H,H,H) groups, {H,H1} of C16 
 At 1.2 times of: 
  {H12A,H12B} of C12, {H8A,H8B} of C8, {H13A,H13B} of C13, {H10A,H10B} of C10, 
   {H6A,H6B} of C6, {H4A,H4B} of C4 
2.a Secondary CH2 refined with riding coordinates: 
 C13(H13A,H13B), C10(H10A,H10B), C12(H12A,H12B), C8(H8A,H8B), C4(H4A,H4B), 
 C6(H6A,H6B) 
2.b Idealised Me refined as rotating group: 
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), 
 C5(H5A,H5B,H5C) 
;
_shelx_res_checksum              8979
_olex2_submission_special_instructions 'No special instructions were received'