Use of Bisulfite Processing To Generate High-β-O-4 Content Water-Soluble Lignosulfonates
Miles-Barrett, Daniel M.; Montgomery, James R. D.; Lancefield, Christopher S.; Cordes, David B.; Slawin, Alexandra M. Z.; Lebl, Tomas; Carr, Reuben; Westwood, Nicholas J.; ACS Sustainable Chemistry & Engineering 5 (2017) 1831–; doi:10.1021/acssuschemeng.6b02566

data_4517008
_publ_section_title
;
 Use of Bisulfite Processing To Generate High-\b-O-4 Content Water-Soluble
 Lignosulfonates
;
_journal_issue                   2
_journal_name_full               'ACS Sustainable Chemistry &amp; Engineering'
_journal_page_first              1831
_journal_paper_doi               10.1021/acssuschemeng.6b02566
_journal_volume                  5
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H23 O8 S, Na, 0.5(C H4 O), 0.5(C3 H6 O)'
_chemical_formula_sum            'C22 H28 Na O9 S'
_chemical_formula_weight         491.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-29
_audit_creation_method           'by CrystalStructure 4.2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.810(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   19.0828(12)
_cell_length_b                   11.0641(5)
_cell_length_c                   21.9710(11)
_cell_measurement_reflns_used    7928
_cell_measurement_temperature    173
_cell_measurement_theta_max      67.68
_cell_measurement_theta_min      4.07
_cell_volume                     4571.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku XtaLAB P100'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23031
_diffrn_reflns_point_group_measured_fraction_full 0.729
_diffrn_reflns_point_group_measured_fraction_max 0.723
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         4.084
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43i (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2072.00
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details
;
 Flack x determined using 1402 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.248(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     617
_refine_ls_number_reflns         6067
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1433P)^2^+0.0214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.462
_reflns_Friedel_fraction_full    0.463
_reflns_Friedel_fraction_max     0.457
_reflns_number_gt                5221
_reflns_number_total             6067
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            sc6b02566_si_005.cif
_cod_data_source_block           S19
_cod_depositor_comments
;

2024-02-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H56 Na2 O18 S2'
_cod_original_formula_weight         983.02
_cod_original_formula_moiety         'C44 H56 Na2 O18 S2'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               4517008
_shelx_res_checksum              23383
_shelx_hkl_checksum              42626