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_4134217
_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'
_chemical_formula_sum            'C23 H29 Fe N4 O2'
_chemical_formula_weight         449.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 142.261(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.4275(18)
_cell_length_b                   20.3332(4)
_cell_length_c                   15.0048(11)
_cell_measurement_reflns_used    22531
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.0730
_cell_measurement_theta_min      2.6540
_cell_volume                     4748.3(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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \f    -25.79 332.43   1.00   20.00 157.73  85.00  73.87    --   358
  2  \f      1.69 320.94   1.00   20.00  42.11  60.00  73.87    --   319
  3  \f     59.56 272.73   1.00   20.00-134.58  85.00  73.87    --   213
  4  \f    -25.79 291.46   1.00   20.00  79.88  90.00  73.87    --   317
  5  \w     56.35 151.35   1.00   20.00    --   83.00  73.87-150.79   95
  6  \w     16.23 154.23   1.00   20.00    --   15.00  73.87   4.21  138
  7  \f    117.10 217.16   1.00   20.00 143.19  95.00  73.87    --   100
  8  \w     60.03 150.03   1.00   20.00    --   63.00  73.87 159.21   90
  9  \w     96.49 223.49   1.00   20.00    --   65.00  73.87-160.79  127
 10  \w     72.42 231.42   1.00   20.00    --   95.00  73.87  89.21  159
 11  \f     65.27 286.44   1.00   20.00  97.45  90.00  73.87    --   221
 12  \f    -10.20 266.02   1.00   20.00  97.89  40.00  73.87    --   276
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1259286000
_diffrn_orient_matrix_UB_12      -0.0425012000
_diffrn_orient_matrix_UB_13      -0.0798930000
_diffrn_orient_matrix_UB_21      -0.0533789000
_diffrn_orient_matrix_UB_22      0.0583133000
_diffrn_orient_matrix_UB_23      -0.0584409000
_diffrn_orient_matrix_UB_31      0.0971464000
_diffrn_orient_matrix_UB_32      -0.0230754000
_diffrn_orient_matrix_UB_33      -0.0004910000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            37079
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        63.650
_diffrn_reflns_theta_max         63.650
_diffrn_reflns_theta_min         2.839
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51098
_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            black
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0482P)^2^+3.3549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6359
_reflns_number_total             7639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13571_si_002.cif
_cod_data_source_block           xral156
_cod_original_cell_volume        4748.3(11)
_cod_database_code               4134217
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C42H48N4O2Fe1
_reflns_odcompleteness_completeness 93.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     65.87
_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(O3) = Uanis(N5)
3.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C42(H42), C40(H40), C26(H26), C8(H8), C3(H3), C10(H10), C19(H19),
 C17(H17), C33(H33)
3.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C12(H12A,H12B,H12C), C21(H21A,H21B,
 H21C), C5(H5A,H5B,H5C), C35(H35A,H35B,H35C), C14(H14A,H14B,H14C), C44(H44A,
 H44B,H44C), C1(H1A,H1B,H1C), C46(H46A,H46B,H46C), C24(H24A,H24B,H24C),
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C36(H36A,H36B,H36C), C45(H45A,H45B,
 H45C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              59099
_shelx_hkl_checksum              94039
_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 1.725
_oxdiff_exptl_absorpt_empirical_full_min 0.655