Crystal structure of a calcium(II)‒pyrroloquinoline quinone (PQQ) complex outside a protein environment
Lumpe, Henning; Mayer, Peter; Daumann, Lena J.; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620014278

data_2022271
_publ_section_title
;
 Crystal structure of a calcium(II)--pyrroloquinoline quinone (PQQ)
 complex outside a protein environment
;
_journal_coeditor_code           YO3076
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620014278
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Ca3 (C14 H3 N2 O8)2 (H2 O1)11], 2H2 O'
_chemical_formula_moiety         'C28 H28 Ca3 N4 O27, 2(H2 O)'
_chemical_formula_sum            'C28 H32 Ca3 N4 O29'
_chemical_formula_weight         1008.81
_chemical_name_common            HL-I-193-B-1
_chemical_name_systematic
'Poly[[undecaaquabis(\m-4,5-dioxo-4,5-dihydro-1<i>H</i>-pyrrolo[2,3-<i>f</i>]quinoline-2,7,9-tricarboxylato)tricalcium(II)] dihydrate]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_block_code                Ca_C14H14N2O8_H2O_xv585_daumann
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90.8440(10)
_cell_angle_beta                 93.1060(10)
_cell_angle_gamma                98.296(2)
_cell_formula_units_Z            2
_cell_length_a                   6.9363(3)
_cell_length_b                   15.9791(7)
_cell_length_c                   16.9786(7)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      27.1180
_cell_measurement_theta_min      2.7010
_cell_volume                     1858.93(14)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      109(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'fixed-chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture TXS'
_diffrn_measurement_method       'mix of phi and omega scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33048
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.868
_diffrn_source                   'rotating anode (TXS)'
_diffrn_source_current           50
_diffrn_source_power             2.5
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         8166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0198P)^2^+1.5469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                7023
_reflns_number_total             8166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yo3076sup1.cif
_cod_data_source_block           I
_cod_database_code               2022271
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              78408
_shelx_res_checksum              88244
_cod_database_fobs_code 2022271