Proton-detected fast-magic-angle spinning NMR of paramagnetic inorganic solids
Blahut, Jan; Benda, Ladislav; Lejeune, Arthur L.; Sanders, Kevin J.; Burcher, Benjamin; Jeanneau, Erwann; Proriol, David; Catita, Leonor; Breuil, Pierre-Alain R.; Quoineaud, Anne-Agathe; Pell, Andrew J.; Pintacuda, Guido; RSC Advances 11 (2021) 29870–29876; doi:10.1039/D1RA04110J

data_7243645
_publ_section_title
;
 Proton-detected fast-magic-angle spinning NMR of paramagnetic inorganic
 solids
;
_journal_issue                   47
_journal_name_full               'RSC Advances'
_journal_page_first              29870
_journal_page_last               29876
_journal_paper_doi               10.1039/D1RA04110J
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C12 H21 Cl2 Fe N2 P'
_chemical_formula_sum            'C12 H21 Cl2 Fe N2 P'
_chemical_formula_weight         351.03
_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             2021-02-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-02-16 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.280(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3959(11)
_cell_length_b                   23.352(2)
_cell_length_c                   11.4368(10)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1260
_cell_measurement_theta_min      3.2520
_cell_volume                     3296.6(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details
;
  1 omega  -64.00   39.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       12.3922  -37.0000  120.0000 103

  2 omega  -14.00   89.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       12.3922   37.0000   90.0000 103

  3 omega  -14.00   89.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       12.3922   37.0000  -60.0000 103

  4 omega   57.00  102.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       12.3922  178.0000  -60.0000 45

  5 omega   57.00  102.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       12.3922  178.0000 -180.0000 45

  6 omega  -17.00   10.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       12.3922   57.0000 -180.0000 27

  7 omega  -64.00  -14.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       12.3922  -37.0000  -60.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0352586000
_diffrn_orient_matrix_UB_12      -0.0002172000
_diffrn_orient_matrix_UB_13      0.0454185000
_diffrn_orient_matrix_UB_21      0.0279553000
_diffrn_orient_matrix_UB_22      -0.0240705000
_diffrn_orient_matrix_UB_23      0.0255483000
_diffrn_orient_matrix_UB_31      0.0357727000
_diffrn_orient_matrix_UB_32      0.0185452000
_diffrn_orient_matrix_UB_33      0.0340267000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38663
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.483
_diffrn_reflns_theta_min         2.902
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.6022
_exptl_crystal_size_mid          0.4825
_exptl_crystal_size_min          0.3905
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         8368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0811P)^2^+7.5940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6789
_reflns_number_total             8368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra04110j2.cif
_cod_data_source_block           numerical
_cod_database_code               7243645
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H21 Cl2 Fe N2 P'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C7(H7), C10(H10), C19(H19), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C13(H13), C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id BB118
_olex2_submission_special_instructions 'No special instructions were received'