Crystal and solution structures of calcium complexes relevant to problematic waste disposal: calcium gluconate and calcium isosaccharinate
Bugris, V.; Dudás, Cs.; Kutus, B.; Harmat, V.; Csankó, K.; Brockhauser, S.; Pálinkó, I.; Turner, Peter; Sipos, P.; Acta Crystallographica Section B 74 (2018) –; doi:10.1107/S2052520618013720

data_2108292
_publ_section_title
;
 Crystal and solution structures of calcium complexes relevant to
 problematic waste disposal: calcium gluconate and calcium isosaccharinate
;
_journal_coeditor_code           BM5106SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520618013720
_journal_volume                  74
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Ca 2+, (C6 H11 O7 1-)2, H2 O'
_chemical_formula_sum            'C12 H24 Ca O15'
_chemical_formula_weight         448.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.71198(9)
_cell_length_b                   13.36410(17)
_cell_length_c                   19.5439(3)
_cell_measurement_reflns_used    35610
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      37.8
_cell_measurement_theta_min      2.1
_cell_volume                     1753.08(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_molecular_graphics
;
  OLEX2 (Dolomanov,O.V.et al., 2009)
  shelXle (H\"ubschle,C.B., et al., 2011)

;
_computing_publication_material
;    
  WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'ShelxT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N, to a short length of fibre supported on a 
thin piece of copper wire inserted in a copper mounting pin on a magnetic 
base.  The crystal was quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;
_diffrn_detector                 'HyPix-6000HE hybrid photon counting detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'AFC12 kappa'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            77828
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.196
_diffrn_reflns_theta_min         1.846
_diffrn_source_type              'Rigaku FRE'
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 3689 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         9212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0233
_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^)+(0.028P)^2^+0.15P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                8854
_reflns_number_total             9212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bm5106sup1.cif
_cod_data_source_block           I
_cod_database_code               2108292
_cod_database_fobs_code          2108292
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.990
_oxdiff_exptl_absorpt_empirical_full_min 0.598
_oxdiff_exptl_absorpt_empirical_full_max 2.62
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              40435
_shelx_hkl_checksum              10378