Electrocatalytic Ammonia Oxidation Mediated by a Polypyridyl Iron Catalyst
Zott, Michael D.; Garrido-Barros, Pablo; Peters, Jonas C.; ACS Catalysis  (2019) 10101–; doi:10.1021/acscatal.9b03499

data_4514891
_publ_section_title
;
 Electrocatalytic Ammonia Oxidation Mediated by a Polypyridyl Iron
 Catalyst
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              10101
_journal_paper_doi               10.1021/acscatal.9b03499
_journal_year                    2019
_chemical_formula_moiety
'4(C18 H24 Fe N6), 8(C F3 O3 S), 3(C4 H8 O), H1.28 N0.43'
_chemical_formula_sum            'C92 H121.28 F24 Fe4 N24.43 O27 S8'
_chemical_formula_weight         2937.24
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.475(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.690(8)
_cell_length_b                   12.063(5)
_cell_length_c                   34.405(5)
_cell_measurement_reflns_used    1986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.17
_cell_measurement_theta_min      2.67
_cell_volume                     12400(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            316748
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.978
_diffrn_reflns_theta_min         2.321
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.952
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1307 before and 0.0930 after correction.
The Ratio of minimum to maximum transmission is 0.6688.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             6033
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.144
_refine_diff_density_max         1.830
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1991
_refine_ls_number_reflns         26746
_refine_ls_number_restraints     2397
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0739
_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^)+(0.0363P)^2^+56.8150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24235
_reflns_number_total             26746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b03499_si_002.cif
_cod_data_source_block           mdz-v19238-final
_cod_original_cell_volume        12399(6)
_cod_database_code               4514891
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 N33-H33A = N33-H33B = N33-H33C
 1.019 with sigma of 0.005
 H33A-H33B = H33A-H33C = H33B-H33C
 1.48 with sigma of 0.01
 N023-C03Z \\sim N0-C03{
 with sigma of 0.02
 N023-C04G \\sim N0-C5AA
 with sigma of 0.02
 N028-C04E \\sim N1-C04F
 with sigma of 0.02
 N028-C04P \\sim N1-C2AA
 with sigma of 0.02
 C02A-N032 \\sim C1AA-N2
 with sigma of 0.02
 C02A-C04P \\sim C1AA-C2AA
 with sigma of 0.02
 C02B-N032 \\sim C3AA-N2
 with sigma of 0.02
 C02B-C04G \\sim C3AA-C5AA
 with sigma of 0.02
 C02H-C045 \\sim C1BA-C0
 with sigma of 0.02
 C02H-C04E \\sim C1BA-C04F
 with sigma of 0.02
 N02T-C03X \\sim N0AA-C6AA
 with sigma of 0.02
 N02T-C04H \\sim N0AA-C7AA
 with sigma of 0.02
 C02X-C03I \\sim C0BA-C4BA
 with sigma of 0.02
 C02X-C04G \\sim C0BA-C5AA
 with sigma of 0.02
 N032-C03Q \\sim N2-C4AA
 with sigma of 0.02
 C03C-C03J \\sim C3BA-C5BA
 with sigma of 0.02
 C03C-C04H \\sim C3BA-C7AA
 with sigma of 0.02
 C03E-C03I \\sim C9AA-C4BA
 with sigma of 0.02
 C03E-C03Z \\sim C9AA-C03{
 with sigma of 0.02
 C03J-C03Y \\sim C5BA-C2BA
 with sigma of 0.02
 C03Q-C04H \\sim C4AA-C7AA
 with sigma of 0.02
 C03W-C045 \\sim C8AA-C0
 with sigma of 0.02
 C03W-C04P \\sim C8AA-C2AA
 with sigma of 0.02
 C03X-C03Y \\sim C6AA-C2BA
 with sigma of 0.02
 N01O-N023 \\sim N01P-N0
 with sigma of 0.04
 N01O-N028 \\sim N01P-N1
 with sigma of 0.04
 N01O-N02P \\sim N01P-N02Q
 with sigma of 0.04
 N01O-N02T \\sim N01P-N0AA
 with sigma of 0.04
 N01O-N032 \\sim N01P-N2
 with sigma of 0.04
 N023-N028 \\sim N0-N1
 with sigma of 0.04
 N023-C02B \\sim N0-C3AA
 with sigma of 0.04
 N023-N02P \\sim N0-N02Q
 with sigma of 0.04
 N023-N02T \\sim N0-N0AA
 with sigma of 0.04
 N023-C02X \\sim N0-C0BA
 with sigma of 0.04
 N023-N032 \\sim N0-N2
 with sigma of 0.04
 N023-C03E \\sim N0-C9AA
 with sigma of 0.04
 N028-C02A \\sim N1-C1AA
 with sigma of 0.04
 N028-C02H \\sim N1-C1BA
 with sigma of 0.04
 N028-N02P \\sim N1-N02Q
 with sigma of 0.04
 N028-N02T \\sim N1-N0AA
 with sigma of 0.04
 N028-N032 \\sim N1-N2
 with sigma of 0.04
 N028-C03W \\sim N1-C8AA
 with sigma of 0.04
 C02A-C02B \\sim C1AA-C3AA
 with sigma of 0.04
 C02A-C03Q \\sim C1AA-C4AA
 with sigma of 0.04
 C02A-C03W \\sim C1AA-C8AA
 with sigma of 0.04
 C02B-C02X \\sim C3AA-C0BA
 with sigma of 0.04
 C02B-C03Q \\sim C3AA-C4AA
 with sigma of 0.04
 C02H-C03W \\sim C1BA-C8AA
 with sigma of 0.04
 N02P-N02T \\sim N02Q-N0AA
 with sigma of 0.04
 N02P-N032 \\sim N02Q-N2
 with sigma of 0.04
 N02T-N032 \\sim N0AA-N2
 with sigma of 0.04
 N02T-C03C \\sim N0AA-C3BA
 with sigma of 0.04
 N02T-C03Q \\sim N0AA-C4AA
 with sigma of 0.04
 N02T-C03Y \\sim N0AA-C2BA
 with sigma of 0.04
 C02X-C03E \\sim C0BA-C9AA
 with sigma of 0.04
 N032-C04G \\sim N2-C5AA
 with sigma of 0.04
 N032-C04H \\sim N2-C7AA
 with sigma of 0.04
 N032-C04P \\sim N2-C2AA
 with sigma of 0.04
 C03C-C03Q \\sim C3BA-C4AA
 with sigma of 0.04
 C03C-C03Y \\sim C3BA-C2BA
 with sigma of 0.04
 C03I-C03Z \\sim C4BA-C03{
 with sigma of 0.04
 C03I-C04G \\sim C4BA-C5AA
 with sigma of 0.04
 C03J-C03X \\sim C5BA-C6AA
 with sigma of 0.04
 C03J-C04H \\sim C5BA-C7AA
 with sigma of 0.04
 C03X-C04H \\sim C6AA-C7AA
 with sigma of 0.04
 C03Z-C04G \\sim C03{-C5AA
 with sigma of 0.04
 C045-C04E \\sim C0-C04F
 with sigma of 0.04
 C045-C04P \\sim C0-C2AA
 with sigma of 0.04
 C04E-C04P \\sim C04F-C2AA
 with sigma of 0.04
 Fe04-N01O \\sim Fe-N01P
 with sigma of 0.02
 Fe04-N023 \\sim Fe-N0
 with sigma of 0.02
 Fe04-N028 \\sim Fe-N1
 with sigma of 0.02
 Fe04-N02P \\sim Fe-N02Q
 with sigma of 0.02
 Fe04-N02T \\sim Fe-N0AA
 with sigma of 0.02
 Fe04-N032 \\sim Fe-N2
 with sigma of 0.02
 Fe04-C02A \\sim Fe-C1AA
 with sigma of 0.04
 Fe04-C02B \\sim Fe-C3AA
 with sigma of 0.04
 Fe04-C03Q \\sim Fe-C4AA
 with sigma of 0.04
 Fe04-C03X \\sim Fe-C6AA
 with sigma of 0.04
 Fe04-C03Z \\sim Fe-C03{
 with sigma of 0.04
 Fe04-C04E \\sim Fe-C04F
 with sigma of 0.04
 Fe04-C04G \\sim Fe-C5AA
 with sigma of 0.04
 Fe04-C04H \\sim Fe-C7AA
 with sigma of 0.04
 Fe04-C04P \\sim Fe-C2AA
 with sigma of 0.04
 S00C-O016 \\sim S00D-O0
 with sigma of 0.02
 S00C-O01E \\sim S00D-O01F
 with sigma of 0.02
 S00C-O01H \\sim S00D-O0AA
 with sigma of 0.02
 S00C-C047 \\sim S00D-C1
 with sigma of 0.02
 F00M-C047 \\sim F00N-C1
 with sigma of 0.02
 F019-C047 \\sim F0-C1
 with sigma of 0.02
 S00C-F00M \\sim S00D-F00N
 with sigma of 0.04
 S00C-F019 \\sim S00D-F0
 with sigma of 0.04
 F00M-F019 \\sim F00N-F0
 with sigma of 0.04
 O016-O01E \\sim O0-O01F
 with sigma of 0.04
 O016-O01H \\sim O0-O0AA
 with sigma of 0.04
 O016-C047 \\sim O0-C1
 with sigma of 0.04
 O01E-O01H \\sim O01F-O0AA
 with sigma of 0.04
 O01E-C047 \\sim O01F-C1
 with sigma of 0.04
 O01H-C047 \\sim O0AA-C1
 with sigma of 0.04
 F01T-C047 \\sim F01U-C1
 with sigma of 0.02
 S00C-F01T \\sim S00D-F01U
 with sigma of 0.04
 F00M-F01T \\sim F00N-F01U
 with sigma of 0.04
 F019-F01T \\sim F0-F01U
 with sigma of 0.04
 N022-C044 \\sim N022-C2
 with sigma of 0.02
 C030-C044 \\sim C030-C2
 with sigma of 0.02
 S00B-O01L \\sim S00B-O01M
 with sigma of 0.02
 S00B-O024 \\sim S00B-O2
 with sigma of 0.02
 S00B-O025 \\sim S00B-O1
 with sigma of 0.02
 O01L-H1AB \\sim O01M-H1AB
 with sigma of 0.02
 F027-C02M \\sim F1-C02M
 with sigma of 0.02
 F02F-C02M \\sim F02G-C02M
 with sigma of 0.02
 C02M-F03M \\sim C02M-F03N
 with sigma of 0.02
 S00A-C04A \\sim S009-C04N \\sim S00B-C02M \\sim S00C-C047 \\sim S00D-C1 \\sim
S005-C040 \\sim S008-
 C03P \\sim S007-C02S \\sim S006-C04B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1BA \\sim Fe \\sim N1 \\sim N0AA \\sim N0 \\sim N02Q \\sim N2 \\sim N01P \\sim
C2AA \\sim C04F \\sim C6AA \\sim C7AA \\sim C03{ \\sim C5AA \\sim H02 \\sim HD
\\sim HE \\sim C1AA \\sim C3AA \\sim C4AA \\sim H01V \\sim H01W \\sim H01X
\\sim C8AA \\sim H04H \\sim H6AA \\sim C2BA \\sim C3BA \\sim H03{ \\sim C9AA
\\sim C0BA \\sim H1AA \\sim H1AB \\sim H3AA \\sim H3AB \\sim H4AA \\sim H4AB
\\sim H8AA \\sim C0 \\sim H1BA \\sim H2BA \\sim C5BA \\sim H3BA \\sim H9AA
\\sim C4BA \\sim H0BA \\sim H0 \\sim H5BA \\sim H4BA \\sim Fe04 \\sim N01O
\\sim N023 \\sim N028 \\sim N02P \\sim N02T \\sim N032 \\sim H01S \\sim H01T
\\sim H01U \\sim C03Z \\sim C04G \\sim C04E \\sim C04P \\sim H02S \\sim H02T
\\sim H02W \\sim C03X \\sim C04H \\sim C02A \\sim C02B \\sim C03Q \\sim C03E
\\sim H03Z \\sim C02X \\sim C02H \\sim H04G \\sim C03W \\sim H03X \\sim C03Y
\\sim C03C \\sim H02N \\sim H02O \\sim H02P \\sim H02Q \\sim H03M \\sim H03P
\\sim H03I \\sim C03I \\sim H02X \\sim H02R \\sim C045 \\sim H03W \\sim C03J
\\sim H03Y \\sim H03H \\sim H03J \\sim H045 \\sim H03K: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
N02Q \\sim Fe \\sim N1 \\sim N0AA \\sim N0 \\sim N2 \\sim N01P \\sim C2AA \\sim
C04F \\sim C6AA \\sim C7AA \\sim C03{ \\sim C5AA \\sim H02 \\sim HD \\sim HE
\\sim C1AA \\sim C3AA \\sim C4AA \\sim H01V \\sim H01W \\sim H01X \\sim C8AA
\\sim H04H \\sim C1BA \\sim H6AA \\sim C2BA \\sim C3BA \\sim H03{ \\sim C9AA
\\sim C0BA \\sim H1AA \\sim H1AB \\sim H3AA \\sim H3AB \\sim H4AA \\sim H4AB
\\sim H8AA \\sim C0 \\sim H1BA \\sim H2BA \\sim C5BA \\sim H3BA \\sim H9AA
\\sim C4BA \\sim H0BA \\sim H0 \\sim H5BA \\sim H4BA \\sim C02A \\sim Fe04
\\sim N01O \\sim N023 \\sim N028 \\sim N02P \\sim N02T \\sim N032 \\sim H01S
\\sim H01T \\sim H01U \\sim C03Z \\sim C04G \\sim C04E \\sim C04P \\sim H02S
\\sim H02T \\sim H02W \\sim C03X \\sim C04H \\sim C02B \\sim C03Q \\sim C03E
\\sim H03Z \\sim C02X \\sim C02H \\sim H04G \\sim C03W \\sim H03X \\sim C03Y
\\sim C03C \\sim H02N \\sim H02O \\sim H02P \\sim H02Q \\sim H03M \\sim H03P
\\sim H03I \\sim C03I \\sim H02X \\sim H02R \\sim C045 \\sim H03W \\sim C03J
\\sim H03Y \\sim H03H \\sim H03J \\sim H045 \\sim H03K: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
F01U \\sim S00D \\sim O0 \\sim O01F \\sim O0AA \\sim C1 \\sim F00N \\sim F0
\\sim F01T \\sim S00C \\sim O016 \\sim O01E \\sim O01H \\sim C047 \\sim F00M
\\sim F019: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C03{, Fe, N1, N0AA, N0, N02Q, N2, N01P, C2AA, C04F, C6AA, C7AA, C5AA, H02, HD,
  HE, C1AA, C3AA, C4AA, H01V, H01W, H01X, C8AA, H04H, C1BA, H6AA, C2BA, C3BA,
 H03{, C9AA, C0BA, H1AA, H1AB, H3AA, H3AB, H4AA, H4AB, H8AA, C0, H1BA, H2BA,
 C5BA, H3BA, H9AA, C4BA, H0BA, H0, H5BA, H4BA, C03W, Fe04, N01O, N023, N028,
 N02P, N02T, N032, H01S, H01T, H01U, C03Z, C04G, C04E, C04P, H02S, H02T, H02W,
 C03X, C04H, C02A, C02B, C03Q, C03E, H03Z, C02X, C02H, H04G, H03X, C03Y, C03C,
 H02N, H02O, H02P, H02Q, H03M, H03P, H03I, C03I, H02X, H02R, C045, H03W, C03J,
 H03Y, H03H, H03J, H045, H03K
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C030, C044, C2, N022
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C02B, Fe04, N01O, N023, N028, N02P, N02T, N032, H01S, H01T, H01U, C03Z, C04G,
 C04E, C04P, H02S, H02T, H02W, C03X, C04H, C02A, C03Q, C03E, H03Z, C02X, C02H,
 H04G, C03W, H03X, C03Y, C03C, H02N, H02O, H02P, H02Q, H03M, H03P, H03I, C03I,
 H02X, H02R, C045, H03W, C03J, H03Y, H03H, H03J, H045, H03K, N02Q, Fe, N1, N0AA,
  N0, N2, N01P, C2AA, C04F, C6AA, C7AA, C03{, C5AA, H02, HD, HE, C1AA, C3AA,
 C4AA, H01V, H01W, H01X, C8AA, H04H, C1BA, H6AA, C2BA, C3BA, H03{, C9AA, C0BA,
 H1AA, H1AB, H3AA, H3AB, H4AA, H4AB, H8AA, C0, H1BA, H2BA, C5BA, H3BA, H9AA,
 C4BA, H0BA, H0, H5BA, H4BA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O01E, S00C, O016, O01H, C047, F00M, F019, F01T, O01F, S00D, O0, O0AA, C1,
 F00N, F0, F01U, O01M, S00B, O1, O024, O025, O01L, O2, C02M, F027, F02F, F03M,
 F1, F03N, F02G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Fe)=Sof(N0)=Sof(N1)=Sof(N0AA)=Sof(N2)=Sof(N02Q)=Sof(H02)=Sof(HD)=Sof(HE)=
 Sof(N01P)=Sof(H01V)=Sof(H01W)=Sof(H01X)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=
 Sof(C2AA)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=
 Sof(C03{)=Sof(H03{)=Sof(C5AA)=Sof(C04F)=Sof(H04H)=Sof(C6AA)=Sof(H6AA)=
 Sof(C7AA)=Sof(C8AA)=Sof(H8AA)=Sof(C9AA)=Sof(H9AA)=Sof(C0BA)=Sof(H0BA)=
 Sof(C1BA)=Sof(H1BA)=Sof(C2BA)=Sof(H2BA)=Sof(C3BA)=Sof(H3BA)=Sof(C0)=Sof(H0)=
 Sof(C4BA)=Sof(H4BA)=Sof(C5BA)=Sof(H5BA)=1-FVAR(1)
 Sof(Fe04)=Sof(N01O)=Sof(H01S)=Sof(H01T)=Sof(H01U)=Sof(N023)=Sof(N028)=
 Sof(C02A)=Sof(H02N)=Sof(H02O)=Sof(C02B)=Sof(H02P)=Sof(H02Q)=Sof(C02H)=
 Sof(H02R)=Sof(N02P)=Sof(H02S)=Sof(H02T)=Sof(H02W)=Sof(N02T)=Sof(C02X)=
 Sof(H02X)=Sof(N032)=Sof(C03C)=Sof(H03H)=Sof(C03E)=Sof(H03I)=Sof(C03I)=
 Sof(H03J)=Sof(C03J)=Sof(H03K)=Sof(C03Q)=Sof(H03M)=Sof(H03P)=Sof(C03W)=
 Sof(H03W)=Sof(C03X)=Sof(H03X)=Sof(C03Y)=Sof(H03Y)=Sof(C03Z)=Sof(H03Z)=
 Sof(C045)=Sof(H045)=Sof(C04E)=Sof(H04G)=Sof(C04G)=Sof(C04H)=Sof(C04P)=FVAR(1)
 Sof(S00D)=Sof(O0)=Sof(O01F)=Sof(O0AA)=Sof(C1)=Sof(F00N)=Sof(F0)=Sof(F01U)=1-
 FVAR(2)
 Sof(S00C)=Sof(F00M)=Sof(O016)=Sof(F019)=Sof(O01E)=Sof(O01H)=Sof(F01T)=
 Sof(C047)=FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=1-FVAR(3)
 Sof(C044)=Sof(H04A)=Sof(H04B)=FVAR(3)
 Sof(O01M)=Sof(F1)=Sof(F03N)=Sof(F02G)=Sof(O1)=Sof(O2)=1-FVAR(4)
 Sof(O01L)=Sof(O024)=Sof(O025)=Sof(F027)=Sof(F02F)=Sof(F03M)=FVAR(4)
 Sof(N33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(5)
6.a Everything fixed:
 H33A, H33B, H33C
6.b Secondary CH2 refined with riding coordinates:
 C02A(H02N,H02O), C02B(H02P,H02Q), C02C(H02A,H02B), C02N(H02G,H02H), C02Q(H02L,
 H02M), C02R(H02C,H02F), C038(H03A,H03B), C03D(H03C,H03D), C03F(H03F,H03G),
 C03G(H03Q,H03T), C03Q(H03M,H03P), C044(H04A,H04B), C04I(H04C,H04D), C04K(H04R,
 H04T), C04L(H04I,H04K), C04O(H04U,H04V), C04R(H04W,H04X), C04T(H04L,H04N),
 C04V(H04Y,H), C04W(H04Z,HA), C04X(H04,HB), C04Y(H04O,H04P), C04Z(H0AA,HC),
 C050(H05A,H05B), C1AA(H1AA,H1AB), C3AA(H3AA,H3AB), C4AA(H4AA,H4AB), C2(H2A,H2B)
6.c Aromatic/amide H refined with riding coordinates:
 C029(H029), C02D(H02D), C02E(H02E), C02H(H02R), C02I(H02I), C02J(H02J),
 C02K(H02K), C02U(H02U), C02V(H02V), C02X(H02X), C02Y(H02Y), C02Z(H02Z),
 C031(H031), C033(H033), C035(H035), C036(H036), C037(H037), C039(H039),
 C03B(H03E), C03C(H03H), C03E(H03I), C03I(H03J), C03J(H03K), C03L(H03L),
 C03N(H03N), C03O(H03O), C03R(H03R), C03S(H03S), C03U(H03U), C03V(H03V),
 C03W(H03W), C03X(H03X), C03Y(H03Y), C03Z(H03Z), C041(H041), C042(H042),
 C043(H043), C045(H045), C046(H046), C048(H048), C049(H049), C04C(H04E),
 C04D(H04F), C04E(H04G), C04J(H04J), C04M(H04M), C04Q(H04Q), C04S(H04S),
 C03{(H03{), C04F(H04H), C6AA(H6AA), C8AA(H8AA), C9AA(H9AA), C0BA(H0BA),
 C1BA(H1BA), C2BA(H2BA), C3BA(H3BA), C0(H0), C4BA(H4BA), C5BA(H5BA)
6.d Idealised Me refined as rotating group:
 N01A(H01G,H01H,H01I), N01B(H01A,H01B,H01C), N01D(H01M,H01N,H01O), N01J(H01J,
 H01K,H01L), N01N(H01P,H01Q,H01R), N01O(H01S,H01T,H01U), N01V(H01D,H01E,H01F),
 N02P(H02S,H02T,H02W), N02Q(H02,HD,HE), N01P(H01V,H01W,H01X)
;
_shelx_res_checksum              73057
_shelx_hkl_checksum              1611
_olex2_submission_special_instructions 'No special instructions were received'