Water-soluble β-aminobisulfonate building blocks for pH and Cu2+indicators
Cardona, Maria A.; Kveder, Marina; Baisch, Ulrich; Probert, Michael R.; Magri, David C.; RSC Adv. 6 (2016) 84712–; doi:10.1039/C6RA17791C

data_7226484
_publ_section_title
;
 Water-soluble \b-aminobisulfonate building blocks for pH and
 Cu2+indicators
;
_journal_issue                   88
_journal_name_full               'RSC Adv.'
_journal_page_first              84712
_journal_paper_doi               10.1039/C6RA17791C
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         '0.25(C40 H68 K8 N4 O32 S8)'
_chemical_formula_sum            'C10 H17 K2 N O8 S2'
_chemical_formula_weight         421.56
_chemical_name_systematic        'phenyl beta-aminobisulfonate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-09
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-09 deposited with the CCDC.
2016-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2498(3)
_cell_length_b                   22.5592(7)
_cell_length_c                   8.7439(3)
_cell_measurement_reflns_used    9526
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.7190
_cell_measurement_theta_min      3.8600
_cell_volume                     1627.32(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega  -33.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   77.0000   30.0000 60

  2 omega   34.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695 -149.0000 -158.0000 26

  3 omega    0.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000    0.0000 73

  4 omega   -9.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   57.0000 -150.0000 76

  5 omega  -51.00   30.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -38.0000 -150.0000 81

  6 omega  -46.00  -14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  123.0000   85.0000 32

  7 omega  -35.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   38.0000  -60.0000 102

  8 omega   -4.00   52.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000  150.0000 56

  9 omega  -16.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000  -30.0000 44

 10 omega  -26.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   86.0000   76.1730 66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0422405000
_diffrn_orient_matrix_UB_12      0.0221314000
_diffrn_orient_matrix_UB_13      -0.0416327000
_diffrn_orient_matrix_UB_21      -0.0338245000
_diffrn_orient_matrix_UB_22      0.0221626000
_diffrn_orient_matrix_UB_23      0.0478907000
_diffrn_orient_matrix_UB_31      0.0667827000
_diffrn_orient_matrix_UB_32      -0.0027726000
_diffrn_orient_matrix_UB_33      0.0505579000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.778
_diffrn_reflns_theta_min         3.395
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3155
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.1822
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0270P)^2^+0.8504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1812
_reflns_number_total             2066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra17791c2.cif
_cod_data_source_block           dcm004_new
_cod_original_cell_volume        1627.33(9)
_cod_database_code               7226484
_chemical_oxdiff_formula         'C10 H8 N1 S2 O6 K2'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 18/06/2014
_olex2_date_sample_submission    03/06/2014
_olex2_submission_original_sample_id DCM004
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method 'acetone, methanol and water'