Taking Solution Proton NMR to Its Extreme: Prediction and Detection of a Hydride Resonance in an Intermediate-Spin Iron Complex.
Ott, Jonas C.; Wadepohl, Hubert; Enders, Markus; Gade, Lutz H.; Journal of the American Chemical Society 140 (2018) 17413–17417; doi:10.1021/jacs.8b11330

data_4133574
_publ_section_title
;
 Taking Solution Proton NMR to Its Extreme: Prediction and Detection of a
 Hydride Resonance in an Intermediate-Spin Iron Complex.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17413
_journal_page_last               17417
_journal_paper_doi               10.1021/jacs.8b11330
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C42 H73 Fe N P2 Si'
_chemical_formula_sum            'C42 H73 Fe N P2 Si'
_chemical_formula_weight         737.89
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_jo19
_audit_creation_date             2018-04-04
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_audit_update_record
'04.04.2018 15:19:55 CEST UTC+02:00  encif 1.82'
_cell_angle_alpha                90
_cell_angle_beta                 111.339(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2359(3)
_cell_length_b                   16.4096(3)
_cell_length_c                   17.4876(3)
_cell_measurement_reflns_used    17085
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.3720
_cell_measurement_theta_min      2.4740
_cell_volume                     4339.71(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2014 (Giacovazzo et al., 2014)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -47.00 -15.00   0.50   15.00    --    4.00 115.00-154.78   64
  2  \w     -4.00  24.00   0.50   15.00    --   28.00  81.00-105.34   56
  3  \w     -5.00  23.00   0.50   15.00    --   28.00  82.00  66.84   56
  4  \w      2.00  28.00   0.50   15.00    --   32.27  78.00 -89.38   52
  5  \w    -40.00  58.00   0.50   15.00    --   32.27 -38.00-120.00  196
  6  \w      7.00 105.00   0.50   15.00    --   32.27  38.00  30.00  196
  7  \w    -37.00  54.00   0.50   15.00    --   32.27 -57.00  60.00  182
  8  \w      7.00 105.00   0.50   15.00    --   32.27  38.00-150.00  196
  9  \w     12.00 101.00   0.50   15.00    --   32.27-143.00-117.00  178
 10  \w      3.00  91.00   0.50   15.00    --   32.27-127.00  52.00  176
 11  \w     12.00 101.00   0.50   15.00    --   32.27  57.00  90.00  178
 12  \w    -20.00  74.00   0.50   15.00    --   32.27 -99.00-120.00  188
 13  \w      2.00 102.00   0.50   15.00    --   32.27  77.00 150.00  200
 14  \w    -37.00  54.00   0.50   15.00    --   32.27 -57.00 120.00  182
 15  \w     12.00 101.00   0.50   15.00    --   32.27  57.00-150.00  178
 16  \w      2.00 102.00   0.50   15.00    --   32.27  77.00-120.00  200
 17  \w    -37.00  54.00   0.50   15.00    --   32.27 -57.00 -60.00  182
 18  \w      2.00  62.00   0.50   15.00    --   32.27  77.00 -30.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0311815000
_diffrn_orient_matrix_UB_12      0.0002613000
_diffrn_orient_matrix_UB_13      -0.0197710000
_diffrn_orient_matrix_UB_21      -0.0017442000
_diffrn_orient_matrix_UB_22      -0.0431577000
_diffrn_orient_matrix_UB_23      -0.0022807000
_diffrn_orient_matrix_UB_31      -0.0349907000
_diffrn_orient_matrix_UB_32      0.0023863000
_diffrn_orient_matrix_UB_33      -0.0387287000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1275
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            166206
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.168
_diffrn_reflns_theta_min         2.145
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         16561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0431P)^2^+1.5974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11011
_reflns_number_total             16561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11330_si_002.cif
_cod_data_source_block           ga_jo19
_cod_original_cell_volume        4339.71(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4133574
_audit_block_refno               3069
_audit_block_usercomment         'JOAD24 yellow plate'
_chemical_oxdiff_formula         'C42 H73 Fe1 N1 P2 Si1'
_chemical_oxdiff_usercomment     'JOAD24 yellow plate'
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.954
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_shelxl_version_number           2018/3
_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.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C11(H11)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.854
_shelx_res_checksum              97065
_cell_oxdiff_length_a            16.2349(3)
_cell_oxdiff_length_b            16.4097(3)
_cell_oxdiff_length_c            17.4868(3)
_cell_oxdiff_angle_alpha         90.0284(15)
_cell_oxdiff_angle_beta          111.3240(17)
_cell_oxdiff_angle_gamma         89.9877(15)
_cell_oxdiff_volume              4339.71(13)
_cell_oxdiff_measurement_reflns_used 17085