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_4134219
_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         'C49 H71 Fe N4 O2 Y'
_chemical_formula_sum            'C49 H71 Fe N4 O2 Y'
_chemical_formula_weight         892.86
_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             2018-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                100.680(4)
_cell_angle_beta                 109.484(5)
_cell_angle_gamma                92.982(4)
_cell_formula_units_Z            4
_cell_length_a                   14.1543(8)
_cell_length_b                   19.3278(8)
_cell_length_c                   21.0046(9)
_cell_measurement_reflns_used    11860
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.4080
_cell_measurement_theta_min      2.5604
_cell_volume                     5283.0(5)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.1179
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29681
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.337
_exptl_absorpt_coefficient_mu    3.941
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.910
_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    1.123
_exptl_crystal_description       rod
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.775
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         18694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12461
_reflns_number_total             18694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13571_si_005.cif
_cod_data_source_block           2018ab119
_cod_database_code               4134219
_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.a Ternary CH refined with riding coordinates:
 C13(H13), C25(H25), C16(H16), C28(H28), C62(H62), C65(H65), C77(H77), C74(H74)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3), C8(H8), C22(H22), C9(H9), C20(H20), C52(H52), C21(H21),
 C57(H57), C69(H69), C58(H58), C70(H70), C71(H71), C59(H59)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C),
 C34(H34A,H34B,H34C), C48(H48A,H48B,H48C), C38(H38A,H38B,H38C), C36(H36A,H36B,
 H36C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C54(H54A,H54B,H54C), C78(H78A,
 H78B,H78C), C30(H30A,H30B,H30C), C50(H50A,H50B,H50C), C44(H44A,H44B,H44C),
 C32(H32A,H32B,H32C), C29(H29A,H29B,H29C), C76(H76A,H76B,H76C), C26(H26A,H26B,
 H26C), C12(H12A,H12B,H12C), C46(H46A,H46B,H46C), C64(H64A,H64B,H64C), C63(H63A,
 H63B,H63C), C24(H24A,H24B,H24C), C61(H61A,H61B,H61C), C66(H66A,H66B,H66C),
 C27(H27A,H27B,H27C), C14(H14A,H14B,H14C), C94(H94A,H94B,H94C), C86(H86A,H86B,
 H86C), C73(H73A,H73B,H73C), C92(H92A,H92B,H92C), C82(H82A,H82B,H82C), C79(H79A,
 H79B,H79C), C98(H98A,H98B,H98C), C84(H84A,H84B,H84C), C75(H75A,H75B,H75C),
 C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C96(H96A,H96B,H96C)
;
_shelx_res_checksum              50568
_shelx_hkl_checksum              46025
_shelx_fab_checksum              35789
_olex2_submission_special_instructions 'No special instructions were received'