Complete denitrification of nitrate and nitrite to N<sub>2</sub> gas by samarium(II) iodide.
Marks, Walker R.; Baumgardner, Douglas F.; Reinheimer, Eric W.; Gilbertson, John D.; Chemical communications (Cambridge, England) 56 (2020) 11441–11444; doi:10.1039/d0cc04115g

data_7127129
_publ_section_title
;
 Complete denitrification of nitrate and nitrite to N<sub>2</sub> gas by
 samarium(II) iodide.
;
_journal_issue                   77
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11441
_journal_page_last               11444
_journal_paper_doi               10.1039/d0cc04115g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C37.6 H94.2 N2 O27 Sm6, 8(I), 2(H2 O0.7), 0.6(H2 O)'
_chemical_formula_sum            'C37.6 H99.4 I8 N2 O29 Sm6'
_chemical_formula_weight         2961.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-30 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.739(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2715(4)
_cell_length_b                   22.8583(6)
_cell_length_c                   14.2693(3)
_cell_measurement_reflns_used    18031
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2580
_cell_measurement_theta_min      2.2210
_cell_volume                     4654.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -70.00  26.00   0.10    2.00    --   19.20 -13.00  30.00  960
  2  \w    -26.00  16.00   0.10    2.00    --   19.20  77.00   0.00  420
  3  \w     34.00 109.00   0.10    2.00    --   19.20  77.00   0.00  750
  4  \w    -25.00 109.00   0.10    2.00    --   19.20  77.00 -60.00 1340
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0249357000
_diffrn_orient_matrix_UB_12      -0.0023577000
_diffrn_orient_matrix_UB_13      -0.0431770000
_diffrn_orient_matrix_UB_21      0.0422028000
_diffrn_orient_matrix_UB_22      0.0047659000
_diffrn_orient_matrix_UB_23      -0.0246213000
_diffrn_orient_matrix_UB_31      0.0083621000
_diffrn_orient_matrix_UB_32      -0.0305866000
_diffrn_orient_matrix_UB_33      -0.0005400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27446
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.122
_diffrn_reflns_theta_max         25.122
_diffrn_reflns_theta_min         2.194
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.433
_exptl_absorpt_correction_T_max  0.174
_exptl_absorpt_correction_T_min  0.067
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.55a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.113
_exptl_crystal_description       block
_exptl_crystal_F_000             2734
_exptl_crystal_size_max          0.614
_exptl_crystal_size_mid          0.492
_exptl_crystal_size_min          0.371
_refine_diff_density_max         1.892
_refine_diff_density_min         -2.263
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         8236
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0001P)^2^+150.0542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7669
_reflns_number_total             8236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04115g2.cif
_cod_data_source_block           er_1
_cod_depositor_comments
'Adding full bibliography for 7127127--7127129.cif.'
_cod_original_formula_sum        'C37.60 H99.40 I8 N2 O29 Sm6'
_cod_database_code               7127129
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C37.6 H86.8 I8 N2 O31 Sm6'
_reflns_odcompleteness_completeness 98.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O13-H13
 0.93 with sigma of 0.02
 O12-H12 = O12_$1-H12_$1
 0.93 with sigma of 0.02
 O11-H11
 0.93 with sigma of 0.01
 H10-O10
 0.85 with sigma of 0.05
 O2A-H2AD = O2A-H2AE
 0.95 with sigma of 0.02
 C4A-C6A \\sim C4B-C6B \\sim C4A-C5A \\sim C4B-C5B
 with sigma of 0.001
 C9B-C7B \\sim C8B-C7B \\sim C9A-C7A \\sim C8A-C7A
 with sigma of 0.001
 C9A-C8A \\sim C9B-C8B
 with sigma of 0.001
 O6-C7A \\sim O6-C7B
 with sigma of 0.001
 C11A-C10B \\sim C11A-C10A \\sim C12B-C10B \\sim C12A-C10A
 with sigma of 0.001
 C11B-C10B \\sim C11A-C10A \\sim C12B-C10B \\sim C12A-C10A
 with sigma of 0.001
 C14A-C13A \\sim C14B-C13B \\sim C15B-C13B \\sim C15A-C13A
 with sigma of 0.001
 O8-C13B \\sim O8-C13A
 with sigma of 0.001
 O2B-C1A \\sim O2C-C1C
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C6A \\sim C4B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C6A \\sim C6B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C4B \\sim C5B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C7A \\sim C7B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C7A \\sim C9B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C7B \\sim C8B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C12B \\sim C12A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C12A \\sim C10A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C10A \\sim C10B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C16: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
C17: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
N1: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
C13A \\sim C13B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C14B \\sim C14A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C15B \\sim C15A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
I3A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
C8B \\sim C9A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C8B \\sim C8A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
H8AC: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C5B \\sim C9B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
I2 \\sim I2A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C5A \\sim C5B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
O2A \\sim O15A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
O15 \\sim O15A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C4B) = Uanis(C4A)
Uanis(C5B) = Uanis(C5A)
Uanis(C7B) = Uanis(C9B)
Uanis(O5) = Uanis(O2A)
Uanis(C18) = Uanis(C2A)
Uanis(C2A) = Uanis(C1A)
Uanis(C2A) = Uanis(C3A)
Uanis(O2A) = Uanis(O2B)
Uanis(O2A) = Uanis(O2C)
Uanis(C3A) = Uanis(C1C)
Uanis(C3A) = Uanis(C2C)
Uanis(C3A) = Uanis(C3C)
Uanis(O3) = Uanis(O15A)
Uanis(O15A) = Uanis(O15)
Uanis(O2B) = Uanis(O15A)
4. Rigid body (RIGU) restrains
 C4A, C5B, C6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5B, C5A, C4B, C5B, C4A, C4B, C6A, C6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C12B, C10B, C11B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C12A, C10A, C11A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C16, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14B, C13B, C15B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14A, C13A, C15A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2B, C1A, C2A, C3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 H17B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C9B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 I1, I1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O10
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O15, H15G, O15A, H15I, H15J
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 H15I, O15A, H15J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H2CA, O15A, H15I, H15J, O15, H15G, H15H
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 I1A, I1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=
 Sof(C4A)=1-FVAR(1)
 Sof(C4B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=
 Sof(H5BC)=FVAR(1)
 Sof(I2A)=1-FVAR(2)
 Sof(I2)=FVAR(2)
 Sof(I1A)=1-FVAR(3)
 Sof(I1)=FVAR(3)
 Sof(O15A)=Sof(H15I)=Sof(H15J)=1-FVAR(4)
 Sof(O15)=FVAR(4)
 Fixed Sof: I3A(0.9) I4B(0.24) C7A(0.9) C13B(0.25) C10A(0.55) C15B(0.25)
 H15A(0.25) H15B(0.25) H15C(0.25) C8A(0.9) H8AA(0.9) H8AB(0.9) H8AC(0.9)
 C14B(0.25) H14A(0.25) H14B(0.25) H14C(0.25) C9A(0.9) H9AA(0.9) H9AB(0.9)
 H9AC(0.9) C1A(0.4) C2A(0.4) H2AA(0.4) H2AB(0.4) H2AC(0.4) C3A(0.4) H3AA(0.4)
 H3AB(0.4) H3AC(0.4) C11A(0.55) H11A(0.55) H11B(0.55) H11C(0.55) I4A(0.76)
 I3B(0.1) O2B(0.4) C7B(0.1) C9B(0.1) C8B(0.1) H8BA(0.1) H8BB(0.1) H8BC(0.1)
 C12B(0.45) H12A(0.45) H12B(0.45) H12C(0.45) C12A(0.55) H12D(0.55) H12E(0.55)
 H12F(0.55) C10B(0.45) C11B(0.45) H11D(0.45) H11E(0.45) H11F(0.45) C15A(0.75)
 H15D(0.75) H15E(0.75) H15F(0.75) C13A(0.75) C14A(0.75) H14D(0.75) H14E(0.75)
 H14F(0.75) O2A(0.4) H2AD(0.4) H2AE(0.4) O2C(0.2) C1C(0.2) C2C(0.2) H2CA(0.2)
 H2CB(0.2) H2CC(0.2) C3C(0.2) H3CA(0.2) H3CB(0.2) H3CC(0.2)
6.a Free rotating group:
 O15A(H15I,H15J)
6.b Rotating group:
 O5(H5A,H5B), O3(H3A,H3B), O1(H1A,H1B), O2A(H2AD,H2AE)
6.c Me refined with riding coordinates:
 C5B(H5BA,H5BB,H5BC), C8B(H8BA,H8BB,H8BC)
6.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C6A(H6AA,H6AB,H6AC), C15B(H15A,H15B,
 H15C), C5A(H5AA,H5AB,H5AC), C8A(H8AA,H8AB,H8AC), C14B(H14A,H14B,H14C),
 C9A(H9AA,H9AB,H9AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C11A(H11A,H11B,
 H11C), C6B(H6BA,H6BB,H6BC), C12B(H12A,H12B,H12C), C12A(H12D,H12E,H12F),
 C11B(H11D,H11E,H11F), C17(H17A,H17B,H17C), C15A(H15D,H15E,H15F), C14A(H14D,
 H14E,H14F), C2C(H2CA,H2CB,H2CC), C3C(H3CA,H3CB,H3CC)
;
_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 2.013
_oxdiff_exptl_absorpt_empirical_full_min 0.539