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_7127127
_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         'C20 H40 I2 O5 Sm, C8 H16 I4 O2 Sm'
_chemical_formula_sum            'C28 H56 I6 O7 Sm2'
_chemical_formula_weight         1566.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-09
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.03.02 svn.r3394 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2020-06-12 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.444(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8008(6)
_cell_length_b                   12.0522(8)
_cell_length_c                   28.7469(16)
_cell_measurement_reflns_used    11618
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      26.5690
_cell_measurement_theta_min      3.2950
_cell_volume                     4386.9(4)
_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                 'Pilatus P200K HPC detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_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    -82.00  75.00   0.10    1.00    --    7.80 -34.00 -54.00 1570
  2  \w    -37.00  97.00   0.10    1.00    --    7.80  77.00 -90.00 1340
  3  \w    -92.00  36.00   0.10    1.00    --   -7.90 -77.00  30.00 1280
;
_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      -0.0519642000
_diffrn_orient_matrix_UB_12      -0.0215412000
_diffrn_orient_matrix_UB_13      -0.0020817000
_diffrn_orient_matrix_UB_21      0.0069943000
_diffrn_orient_matrix_UB_22      -0.0101400000
_diffrn_orient_matrix_UB_23      0.0245992000
_diffrn_orient_matrix_UB_31      -0.0196884000
_diffrn_orient_matrix_UB_32      0.0537555000
_diffrn_orient_matrix_UB_33      0.0037846000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            20025
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.523
_diffrn_reflns_theta_min         3.008
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.908
_exptl_absorpt_correction_T_max  0.400
_exptl_absorpt_correction_T_min  0.045
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.726
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.149
_refine_diff_density_max         2.654
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0543P)^2^+51.2395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4259
_reflns_number_total             4475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04115g2.cif
_cod_data_source_block           20200317_sarmarium_2
_cod_depositor_comments
'Adding full bibliography for 7127127--7127129.cif.'
_cod_database_code               7127127
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C14 H28 I3 O3.5 Sm'
_chemical_oxdiff_usercomment     'Yellow Samarium crystal'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Rigid body (RIGU) restrains
 C2, Sm1, O1, O3, O2, I1, C1, C4, C9, C8, C5, H1A, H1B, H4A, H4B, C3, H9A, H9B,
  C10, H8A, H8B, C7, H5A, H5B, C6, H2A, H2B, H3A, H3B, H10A, H10B, H7A, H7B,
 H6A, H6B, Sm1, O1, Sm1, O3, Sm1, O2, Sm1, I1, O1, C1, O1, C4, O3, C9, O2, C8,
 O2, C5, C1, H1A, C1, H1B, C2, C1, C4, H4A, C4, H4B, C3, C4, C9, H9A, C9, H9B,
 C10, C9, C8, H8A, C8, H8B, C7, C8, C5, H5A, C5, H5B, C6, C5, C2, H2A, C2, H2B,
 C3, C2, C3, H3A, C3, H3B, C10, H10A, C10, H10B, C7, H7A, C7, H7B, C6, C7, C6,
 H6A, C6, H6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C14(H14A,H14B), C9(H9A,H9B), C1(H1A,H1B), C4(H4A,H4B), C8(H8A,
 H8B), C12(H12A,H12B), C13(H13A,H13B), C5(H5A,H5B), C7(H7A,H7B), C2(H2A,H2B),
 C10(H10A,H10B), C3(H3A,H3B), C6(H6A,H6B)
;
_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 7.343
_oxdiff_exptl_absorpt_empirical_full_min 0.495