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_2108293
_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 O6 1-)2'
_chemical_formula_sum            'C12 H22 Ca O12'
_chemical_formula_weight         398.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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            2
_cell_length_a                   6.7573(4)
_cell_length_b                   19.5874(10)
_cell_length_c                   5.7344(10)
_cell_measurement_reflns_used    3861
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.27
_cell_volume                     758.99(15)
_computing_data_collection
' mxCuBE v2 (Gabadinho et al. 2010, JSR, 27, 700-707)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics
;
  OLEX2 (Dolomanov,O.V.et al., 2009)
  shelXle (H\"ubschle,C.B., et al., 2011)
;
_computing_publication_material
;    
  WinGX (Farrugia, 1999)
  PWT (Farrugia, 2013)
  PLATON (Spek, A.K., 2003) 
  XNPP (Parsons, S., et al., 2013)   ##?? 
;
_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 nylon loop and quenched 
in a cold nitrogen gas stream from an Oxford Cryojet. 
;
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device       'Pilatus 6M-F (25 Hz) and MD2 mini-kappa'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'EMBL PETRA III P13-MX1 beamline'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4539
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         28.522
_diffrn_reflns_theta_min         2.267
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       needle
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 541 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.050(19)
_refine_ls_extinction_coef       0.180(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1394
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0333
_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^)+(0.03P)^2^+0.3P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.634
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                1393
_reflns_number_total             1394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bm5106sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        758.99(14)
_cod_database_code               2108293
_cod_database_fobs_code          2108293
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              40461
_shelx_hkl_checksum              29305