Organosolv processing of Sitka spruce sawdust: large scale preparation of native-like lignin and lignin<sup>OX</sup> for valorisation.
Davidson, Daniel J.; Sansom, Geraud N.; Miles-Barrett, Daniel M; Cordes, David B.; Slawin, Alexandra M. Z.; Montgomery, James R. D.; Lebl, Tomas; Connor, Ann; Danby, Andrew M.; Gronnow, Mark J.; Parry, Neil J.; Hosking, Sarah L.; Grainger, David S.; Westwood, Nicholas J.; Faraday discussions 263 (2026) 98–122; doi:10.1039/d5fd00074b

data_1574876
_publ_section_title
;
 Organosolv processing of Sitka spruce sawdust: large scale preparation of
 native-like lignin and lignin<sup>OX</sup> for valorisation.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              98
_journal_page_last               122
_journal_paper_doi               10.1039/d5fd00074b
_journal_volume                  263
_journal_year                    2026
_chemical_formula_moiety         'C24 H24 O9'
_chemical_formula_sum            'C24 H24 O9'
_chemical_formula_weight         456.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-04-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-21 deposited with the CCDC.	2025-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                78.835(11)
_cell_angle_beta                 87.376(12)
_cell_angle_gamma                88.318(13)
_cell_formula_units_Z            2
_cell_length_a                   9.885(2)
_cell_length_b                   10.504(3)
_cell_length_c                   10.763(3)
_cell_measurement_reflns_used    1661
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.0
_cell_volume                     1095.0(5)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'hybrid photon counting detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Dectris PILATUS P200K'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -100.0000 - 80.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.1120
	          2theta: -10.0143
scan:
	Number of images: 360
	           Slice: -100.0000 - 80.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.1120
	          2theta: -10.0143
scan:
	Number of images: 360
	           Slice: -100.0000 - 80.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.1120
	          2theta: -10.0143
;
_diffrn_measurement_device       'AFC10: Fixed \c 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200K'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support Loop
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.013741
_diffrn_orient_matrix_UB_12      -0.097597
_diffrn_orient_matrix_UB_13      0.023363
_diffrn_orient_matrix_UB_21      -0.091158
_diffrn_orient_matrix_UB_22      -0.002778
_diffrn_orient_matrix_UB_23      0.033216
_diffrn_orient_matrix_UB_31      -0.013382
_diffrn_orient_matrix_UB_32      -0.019818
_diffrn_orient_matrix_UB_33      -0.091717
_diffrn_radiation_monochromator  'Rigaku Osmic Confocal Optical System'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13488
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.388
_diffrn_reflns_theta_min         1.930
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           66.0
_diffrn_source_power             3.0
_diffrn_source_type              'Rigaku FR-X'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             480
_exptl_crystal_preparation       Loop
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/petroleum ether/diethyl ether'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.4007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2691
_reflns_number_total             3972
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d5fd00074b2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1574876.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1574876
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C11(H11), C15(H15), C18(H18), C22(H22)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              3604
_shelx_hkl_checksum              98293