Crystal structure and bonding analysis of the first dinuclear calcium(II)–proton-pump inhibitor (PPI) `butterfly molecule': a combined microcrystal synchrotron and DFT study
Cong, Hengjiang; Acta Crystallographica Section C 72 (2016) 326–336; doi:10.1107/S2053229616004216

data_2020443
_publ_section_title
;
 Crystal structure and bonding analysis of the first dinuclear
 calcium(II)--proton-pump inhibitor (PPI) `butterfly molecule': a combined
 microcrystal synchrotron and DFT study
;
_journal_coeditor_code           LF3028
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              326
_journal_page_last               336
_journal_paper_doi               10.1107/S2053229616004216
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Ca2 (C20 H22 N3 S1 O4)4 (C1 H4 O1)4], 6C1 H4 O1'
_chemical_formula_moiety         'C84 H104 Ca2 N12 O20 S4, 6C1 H4 O1'
_chemical_formula_sum            'C90 H128 Ca2 N12 O26 S4'
_chemical_formula_weight         2002.44
_chemical_name_systematic
'Bis[\m-(<i>R</i>)-2-({[4-(3-methoxypropoxy)-3-methylpyridin-2-yl]methyl}sulfinyl)-6,7-dihydro-3<i>H</i>-benzofuro[5,6-<i>d</i>]imidazol-1-ido]bis{dimethanol[(<i>R</i>)-2-({[4-(3-methoxypropoxy)-3-methylpyridin-2-yl]methyl}sulfinyl)-6,7-dihydro-3<i>H</i>-benzofuro[5,6-<i>d</i>]imidazol-1-ido]calcium(II)} methanol hexasolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.70(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.100(6)
_cell_length_b                   10.560(2)
_cell_length_c                   15.800(3)
_cell_measurement_reflns_used    3062
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.795
_cell_measurement_theta_min      2.895
_cell_volume                     5010.1(19)
_computing_cell_refinement
;
XDS (Kabsch, 2010)
;
_computing_data_collection
;
ADSC Quantum Q315r software
;
_computing_data_reduction
;
XDS (Kabsch, 2010)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'ADSC Q315r CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79987
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39409
_diffrn_reflns_theta_full        28.680
_diffrn_reflns_theta_max         32.795
_diffrn_reflns_theta_min         2.895
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.355
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 5262 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.049(4)
_refine_ls_extinction_coef       0.0096(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         11723
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0536P)^2^+2.6948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                11544
_reflns_number_total             11723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3028sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020443.cif.'
_cod_original_cell_volume        5010(2)
_cod_database_code               2020443
_cod_database_fobs_code          2020443
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.996
_shelx_hkl_checksum              10858
_shelx_res_checksum              18869