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_4134218
_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         'C43 H59 Fe N4 O2 Y'
_chemical_formula_sum            'C43 H59 Fe N4 O2 Y'
_chemical_formula_weight         808.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.66170(10)
_cell_length_b                   21.20880(10)
_cell_length_c                   22.79760(10)
_cell_measurement_reflns_used    17734
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.0270
_cell_measurement_theta_min      3.8800
_cell_volume                     4188.02(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_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    -19.00   6.00   1.00    3.25    --    5.00  30.00 116.00   25
  2  \w   -170.00-143.00   1.00    3.25    --  -89.00  30.00 116.00   27
  3  \w    -88.00  34.00   1.00    1.00    --    0.00  60.00-120.00  122
  4  \w   -151.00 -74.00   1.00    3.25    --  -89.00  43.00-180.00   77
  5  \w    -62.00 -35.00   1.00    3.25    --  -89.00  43.00-180.00   27
  6  \w   -157.00 -71.00   1.00    3.25    --  -89.00  60.00-120.00   86
  7  \w    -41.00 -14.00   1.00    3.25    --  -89.00  60.00-120.00   27
  8  \w    -53.00  -3.00   1.00    3.25    --  -89.00  57.00-150.00   50
  9  \w   -160.00-135.00   1.00    3.25    --  -89.00  60.00 150.00   25
 10  \w    -81.00  -1.00   1.00    3.25    --  -89.00  60.00 150.00   80
 11  \w   -178.00 -18.00   1.00    3.25    --  -89.00  60.00  90.00  160
 12  \w   -173.00-129.00   1.00    3.25    --  -89.00  57.00 -30.00   44
 13  \w   -176.00 -73.00   1.00    3.25    --  -89.00  57.00-150.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27048
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.278
_diffrn_reflns_theta_min         2.846
_exptl_absorpt_coefficient_mu    4.919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       rod
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 3114 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0132(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         7576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0440P)^2^+1.2251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                7405
_reflns_number_total             7576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13571_si_004.cif
_cod_data_source_block           ab_95y
_cod_database_code               4134218
_shelx_shelxl_version_number     2014/7
_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. Uiso/Uaniso restraints and constraints
Uanis(C34) = Uanis(C35) = Uanis(C41) = Uanis(C42) = Uanis(C45) = Uanis(C46)
Uanis(C38) = Uanis(C52) = Uanis(C47) = Uanis(C48)
3. Others
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C42)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C45)=Sof(C50)=Sof(H50A)=
 Sof(H50B)=Sof(H50C)=Sof(C52)=Sof(C47)=Sof(H44D)=Sof(H47A)=Sof(H47B)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C41)=Sof(C46)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C44)=Sof(H44A)=
 Sof(H44B)=Sof(H44C)=Sof(C38)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C20(H20), C17(H17), C8(H8)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C22(H22A,H22B,H22C),
 C27(H27A,H27B,H27C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C33(H33A,H33B,
 H33C), C24(H24A,H24B,H24C), C10(H10A,H10B,H10C), C31(H31A,H31B,H31C), C19(H19A,
 H19B,H19C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C),
 C49(H49A,H49B,H49C), C44(H44A,H44B,H44C), C35(H35A,H35B,H35C), C39(H39A,H39B,
 H39C), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C), C47(H44D,H47A,H47B), C48(H48A,
 H48B,H48C)
;
_shelx_res_checksum              54807
_shelx_hkl_checksum              43327
_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
;