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_4134221
_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 Gd N4 O2'
_chemical_formula_sum            'C43 H59 Fe Gd N4 O2'
_chemical_formula_weight         877.04
_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
_atom_sites_solution_primary     dual
_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                   8.6849(2)
_cell_length_b                   21.2561(3)
_cell_length_c                   22.8285(4)
_cell_measurement_reflns_used    12064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.2060
_cell_measurement_theta_min      3.2400
_cell_volume                     4214.30(14)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18766
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         6.404
_exptl_absorpt_coefficient_mu    13.118
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.478
_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    1.382
_exptl_crystal_description       rod
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.854
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 2625 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0381
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    0.945
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                6842
_reflns_number_total             7360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13571_si_007.cif
_cod_data_source_block           mesFe(NO)2Gd(CpMe5)2
_cod_database_code               4134221
_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(C50) = Uanis(C51) = Uanis(C47) = Uanis(C48) = Uanis(C45) = Uanis(C46) =
Uanis(C41) = Uanis(C42) = Uanis(C37) = Uanis(C38) = Uanis(C35) = Uanis(C36)
3. Others
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C38)=Sof(C42)=Sof(C44)=Sof(H44A)=
 Sof(H44B)=Sof(H44C)=Sof(C46)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=1-FVAR(1)
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C37)=Sof(C41)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(H43C)=Sof(C45)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C17(H17), C8(H8), C19(H19), C3(H3)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C),
 C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C22(H22A,
 H22B,H22C), C33(H33A,H33B,H33C), C50(H50A,H50B,H50C), C35(H35A,H35B,H35C),
 C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C51(H51A,H51B,
 H51C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C48(H48A,
 H48B,H48C)
;
_shelx_res_checksum              1923
_shelx_hkl_checksum              82848
_olex2_submission_special_instructions 'No special instructions were received'