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_4134220
_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         '2(C49 H71 Fe Gd N4 O2), 2(C5 H12)'
_chemical_formula_sum            'C108 H166 Fe2 Gd2 N8 O4'
_chemical_formula_weight         2066.68
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                100.408(2)
_cell_angle_beta                 109.137(2)
_cell_angle_gamma                93.002(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1740(3)
_cell_length_b                   19.2468(4)
_cell_length_c                   20.8800(4)
_cell_measurement_reflns_used    21138
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.0330
_cell_measurement_theta_min      2.2850
_cell_volume                     5254.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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     18.00  56.00   1.00    2.50    --    0.00  60.00-180.00   38
  2  \w    -84.00  76.00   1.00   13.00    --    5.00  60.00 -60.00  160
  3  \w    -87.00 -49.00   1.00   13.00    --  -89.00  60.00 -60.00   38
  4  \w   -158.00-131.00   1.00   13.00    --  -89.00  60.00 120.00   27
  5  \w   -124.00 -10.00   1.00   13.00    --  -89.00  60.00 120.00  114
  6  \w   -177.00-146.00   1.00   13.00    --  -89.00  60.00  30.00   31
  7  \w    -97.00 -11.00   1.00   13.00    --  -89.00  60.00  60.00   86
  8  \w   -171.00  -6.00   1.00   13.00    --  -89.00  60.00  90.00  165
  9  \w   -176.00 -76.00   1.00   13.00    --  -89.00  60.00-150.00  100
 10  \w    -55.00 -26.00   1.00   13.00    --  -89.00  60.00-150.00   29
 11  \w   -168.00-143.00   1.00   13.00    --  -89.00  60.00 150.00   25
 12  \w   -127.00  -1.00   1.00   13.00    --  -89.00  60.00 150.00  126
 13  \w   -165.00-139.00   1.00   13.00    --  -89.00  60.00  60.00   26
 14  \w   -102.00 -17.00   1.00   13.00    --  -89.00  60.00  30.00   85
 15  \w   -118.00 -26.00   1.00   13.00    --  -89.00  57.00-180.00   92
 16  \w   -173.00-102.00   1.00   13.00    --  -89.00  60.00 -60.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0614895000
_diffrn_orient_matrix_UB_12      -0.0721330000
_diffrn_orient_matrix_UB_13      -0.0409047000
_diffrn_orient_matrix_UB_21      -0.0272878000
_diffrn_orient_matrix_UB_22      0.0283298000
_diffrn_orient_matrix_UB_23      -0.0674599000
_diffrn_orient_matrix_UB_31      0.0943610000
_diffrn_orient_matrix_UB_32      -0.0267223000
_diffrn_orient_matrix_UB_33      -0.0124778000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49637
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         2.291
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'intense brown'
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1154
_refine_ls_number_reflns         18556
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0416P)^2^+3.3794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16388
_reflns_number_total             18556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13571_si_008.cif
_cod_data_source_block           2018ab123
_cod_database_code               4134220
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C216 H330 Fe4 Gd4 N16 O8 '
_reflns_odcompleteness_completeness 99.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C101-C102
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C106) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C107) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C112) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C111) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C104) = Uanis(C109) = Uanis(C105) = Uanis(C110) = Uanis(C106) =
Uanis(C111) = Uanis(C107) = Uanis(C112) = Uanis(C108) = Uanis(C113)
4. Rigid body (RIGU) restrains
 C99, C100, C101, C102, C103, C100, C99, C100, C101, C102, C101, C102, C103
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C106(0.7) H10J(0.7) H10K(0.7) C105(0.7) H10L(0.7) H10M(0.7)
 C107(0.7) H10N(0.7) H10O(0.7) C108(0.7) H10P(0.7) H10Q(0.7) H10R(0.7)
 C104(0.7) H10S(0.7) H10T(0.7) H10U(0.7) C112(0.3) H11A(0.3) H11B(0.3)
 C109(0.3) H10V(0.3) H10W(0.3) H10X(0.3) C113(0.3) H11C(0.3) H11D(0.3)
 H11E(0.3) C110(0.3) H11F(0.3) H11G(0.3) C111(0.3) H11H(0.3) H11I(0.3)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C65(H65), C74(H74), C61(H61), C28(H28), C77(H77), C25(H25), C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C100(H10F,H10G), C102(H10H,H10I), C106(H10J,H10K), C105(H10L,
 H10M), C107(H10N,H10O), C112(H11A,H11B), C110(H11F,H11G), C111(H11H,H11I)
6.c Aromatic/amide H refined with riding coordinates:
 C52(H52), C59(H59), C71(H71), C58(H58), C57(H57), C22(H22), C70(H70),
 C21(H21), C20(H20), C69(H69), C10(H10), C8(H8), C3(H3), C9(H9)
6.d Idealised Me refined as rotating group:
 C96(H96A,H96B,H96C), C50(H50A,H50B,H50C), C14(H14A,H14B,H14C), C63(H63A,H63B,
 H63C), C54(H54A,H54B,H54C), C79(H79A,H79B,H79C), C5(H5A,H5B,H5C), C82(H82A,
 H82B,H82C), C89(H89A,H89B,H89C), C64(H64A,H64B,H64C), C92(H92A,H92B,H92C),
 C94(H94A,H94B,H94C), C88(H88A,H88B,H88C), C33(H33A,H33B,H33C), C66(H66A,H66B,
 H66C), C1(H1A,H1B,H1C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C40(H40A,
 H40B,H40C), C98(H98A,H98B,H98C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C),
 C76(H76A,H76B,H76C), C49(H49A,H49B,H49C), C73(H73A,H73B,H73C), C12(H12A,H12B,
 H12C), C43(H43A,H43B,H43C), C75(H75A,H75B,H75C), C27(H27A,H27B,H27C), C47(H47A,
 H47B,H47C), C78(H78A,H78B,H78C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C),
 C36(H36A,H36B,H36C), C62(H62A,H62B,H62C), C26(H26A,H26B,H26C), C45(H45A,H45B,
 H45C), C15(H15A,H15B,H15C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C99(H99A,
 H99B,H99C), C103(H10C,H10D,H10E), C108(H10P,H10Q,H10R), C104(H10S,H10T,H10U),
 C109(H10V,H10W,H10X), C113(H11C,H11D,H11E)
;
_shelx_res_checksum              91687
_shelx_hkl_checksum              79168
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.761
_oxdiff_exptl_absorpt_empirical_full_min 0.335