Coupling of Nitric Oxide and Release of Nitrous Oxide from Rare-Earth-Dinitrosyliron Complexes.
Bar, Arun K.; Heras Ojea, María José; Tang, Jinkui; Layfield, Richard A.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13571

data_4134222
_publ_section_title
;
 Coupling of Nitric Oxide and Release of Nitrous Oxide from
 Rare-Earth-Dinitrosyliron Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13571
_journal_year                    2020
_chemical_formula_moiety         'C23 H29 Fe N4 O2, C16 H36 N'
_chemical_formula_sum            'C39 H65 Fe N5 O2'
_chemical_formula_weight         691.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                100.604(4)
_cell_angle_beta                 111.178(4)
_cell_angle_gamma                91.002(4)
_cell_formula_units_Z            2
_cell_length_a                   11.5668(5)
_cell_length_b                   12.4022(5)
_cell_length_c                   15.0090(8)
_cell_measurement_reflns_used    4371
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      27.0040
_cell_measurement_theta_min      3.3440
_cell_volume                     1965.10(17)
_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  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.985
_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    -56.00  49.00   1.00   12.50    --  -19.95  77.00   0.00  105
  2  \w    -11.00  95.00   1.00   12.50    --   21.12  77.00 120.00  106
  3  \w    -13.00  93.00   1.00   12.50    --   21.12  77.00-120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0579265000
_diffrn_orient_matrix_UB_12      -0.0231142000
_diffrn_orient_matrix_UB_13      0.0103899000
_diffrn_orient_matrix_UB_21      -0.0304187000
_diffrn_orient_matrix_UB_22      -0.0527913000
_diffrn_orient_matrix_UB_23      -0.0070737000
_diffrn_orient_matrix_UB_31      -0.0089800000
_diffrn_orient_matrix_UB_32      -0.0096427000
_diffrn_orient_matrix_UB_33      -0.0502225000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9528
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.645
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0723P)^2^+1.5731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5774
_reflns_number_total             7075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13571_si_003.cif
_cod_data_source_block           aral686
_cod_database_code               4134222
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C50H60N5O2Fe1
_chemical_oxdiff_usercomment     AB75
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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:
 C36(H36A,H36B), C27(H27A,H27B), C37(H37A,H37B), C31(H31A,H31B), C33(H33A,
 H33B), C34(H34A,H34B), C30(H30A,H30B), C38(H38A,H38B), C32(H32A,H32B),
 C29(H29A,H29B), C26(H26A,H26B), C25(H25A,H25B)
2.b Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C5(H5A,H5B,
 H5C), C13(H13A,H13B,H13C), C35(H35A,H35B,H35C), C1(H1A,H1B,H1C), C21(H21A,H21B,
 H21C), C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C39(H39A,H39B,H39C), C24(H24A,
 H24B,H24C)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C19(H19), C17(H17), C10(H10)
;
_shelx_res_checksum              48450
_shelx_hkl_checksum              4850
_olex2_date_sample_data_collection 2018-01-25
_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 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.709