 
data_20190731zju_gld1_0m_a
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C44 H16 Ca8 O40' 
_chemical_formula_weight          1505.21

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ca'  'Ca'   0.2262   0.3064
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            43
_space_group_name_H-M_alt         'F d d 2'
_space_group_name_Hall            'F 2 -2d'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-x+1/4, y+1/4, z+1/4'
 'x+3/4, -y+3/4, z+1/4'
 'x, y+1/2, z+1/2'
 '-x, -y+1/2, z+1/2'
 '-x+1/4, y+3/4, z+3/4'
 'x+3/4, -y+5/4, z+3/4'
 'x+1/2, y, z+1/2'
 '-x+1/2, -y, z+1/2'
 '-x+3/4, y+1/4, z+3/4'
 'x+5/4, -y+3/4, z+3/4'
 'x+1/2, y+1/2, z'
 '-x+1/2, -y+1/2, z'
 '-x+3/4, y+3/4, z+1/4'
 'x+5/4, -y+5/4, z+1/4'
 
_cell_length_a                    19.916(4)
_cell_length_b                    18.697(4)
_cell_length_c                    7.6700(16)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      2856.1(10)
_cell_formula_units_Z             2
_cell_measurement_temperature     193(2)
_cell_measurement_reflns_used      3679
_cell_measurement_theta_min        2.99
_cell_measurement_theta_max       25.27
 
_exptl_crystal_description        'BLOCK'
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.750          
_exptl_crystal_F_000              1520
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.120
_exptl_crystal_size_mid           0.090
_exptl_crystal_size_min           0.060
_exptl_absorpt_coefficient_mu     0.850
_shelx_estimated_absorpt_T_min    0.905
_shelx_estimated_absorpt_T_max    0.951
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       193(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             4280
_diffrn_reflns_av_unetI/netI      0.0418
_diffrn_reflns_av_R_equivalents   0.0530
_diffrn_reflns_limit_h_min        -23
_diffrn_reflns_limit_h_max        21
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        22
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          2.989
_diffrn_reflns_theta_max          25.000
_diffrn_reflns_theta_full         25.000
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.972
_diffrn_reflns_point_group_measured_fraction_full  0.972
_reflns_number_total              1225
_reflns_number_gt                 1187
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.799
_reflns_Friedel_fraction_max      0.940
_reflns_Friedel_fraction_full     0.940
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0997P)²+18.4712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.11(12)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          1225
_refine_ls_number_parameters      107
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0555
_refine_ls_R_factor_gt            0.0544
_refine_ls_wR_factor_ref          0.1421
_refine_ls_wR_factor_gt           0.1406
_refine_ls_goodness_of_fit_ref    1.072
_refine_ls_restrained_S_all       1.071
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ca1 Ca -0.02612(6) 0.27902(6) 0.0398(2) 0.0144(4) Uani 1 1 d . . . . .
O1 O 0.0683(3) 0.3482(3) 0.0818(6) 0.0259(13) Uani 1 1 d . . . . .
O2 O 0.1942(3) 0.4633(3) 0.0918(6) 0.0196(12) Uani 1 1 d . . . . .
O3 O 0.2113(3) 0.4430(3) 0.4860(6) 0.0206(12) Uani 1 1 d . . . . .
O4 O 0.0919(3) 0.3211(3) 0.4967(6) 0.0261(13) Uani 1 1 d . . . . .
O5 O -0.1070(3) 0.3695(4) 0.0431(10) 0.0403(15) Uani 1 1 d . . . . .
H18B H -0.091664 0.406848 -0.006726 0.060 Uiso 1 1 d R U . . .
H18A H -0.141954 0.355528 -0.006956 0.060 Uiso 1 1 d R U . . .
C1 C 0.1079(4) 0.3719(4) 0.1958(9) 0.0165(15) Uani 1 1 d . . . . .
C2 C 0.1180(4) 0.3610(4) 0.3835(9) 0.0173(15) Uani 1 1 d . . . . .
C3 C 0.1716(4) 0.4141(4) 0.3818(10) 0.0188(16) Uani 1 1 d . . . . .
C4 C 0.1629(4) 0.4241(4) 0.1970(9) 0.0173(16) Uani 1 1 d . . . . .
C6 C 0.250000 0.250000 0.244(7) 0.105(14) Uani 1 2 d S T P A 1
C7 C 0.250000 0.250000 0.411(6) 0.109(12) Uani 1 2 d S T P A 1
C5 C 0.250000 0.250000 0.061(6) 0.109(12) Uani 1 2 d S T P A 1
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ca1 O1 2.306(5) . ?
Ca1 O4 2.308(5) 6_554 ?
Ca1 O5 2.336(6) . ?
Ca1 O2 2.395(5) 4_455 ?
Ca1 O3 2.401(5) 4_454 ?
Ca1 O2 2.544(5) 7_544 ?
Ca1 O3 2.553(5) 7_544 ?
Ca1 C4 3.072(7) 7_544 ?
Ca1 C3 3.073(8) 7_544 ?
Ca1 Ca1 4.1191(12) 6 ?
Ca1 Ca1 4.1192(11) 6_554 ?
Ca1 H18B 2.7465 . ?
Ca1 H18A 2.7379 . ?
O1 C1 1.258(9) . ?
O2 C4 1.256(9) . ?
O3 C3 1.247(9) . ?
O4 C2 1.258(9) . ?
O5 H18B 0.8530 . ?
O5 H18A 0.8364 . ?
C1 C2 1.468(9) . ?
C1 C4 1.468(10) . ?
C2 C3 1.458(10) . ?
C3 C4 1.440(9) . ?
C6 C7 1.28(5) . ?
C6 C5 1.40(6) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 Ca1 O4 159.7(2) . 6_554 ?
O1 Ca1 O5 98.9(2) . . ?
O4 Ca1 O5 101.4(2) 6_554 . ?
O1 Ca1 O2 91.85(19) . 4_455 ?
O4 Ca1 O2 92.70(18) 6_554 4_455 ?
O5 Ca1 O2 77.1(2) . 4_455 ?
O1 Ca1 O3 95.63(19) . 4_454 ?
O4 Ca1 O3 88.79(18) 6_554 4_454 ?
O5 Ca1 O3 77.3(2) . 4_454 ?
O2 Ca1 O3 154.15(17) 4_455 4_454 ?
O1 Ca1 O2 80.29(18) . 7_544 ?
O4 Ca1 O2 83.51(18) 6_554 7_544 ?
O5 Ca1 O2 143.0(2) . 7_544 ?
O2 Ca1 O2 139.82(14) 4_455 7_544 ?
O3 Ca1 O2 65.99(16) 4_454 7_544 ?
O1 Ca1 O3 81.89(18) . 7_544 ?
O4 Ca1 O3 81.97(18) 6_554 7_544 ?
O5 Ca1 O3 143.0(2) . 7_544 ?
O2 Ca1 O3 65.92(15) 4_455 7_544 ?
O3 Ca1 O3 139.65(14) 4_454 7_544 ?
O2 Ca1 O3 73.95(15) 7_544 7_544 ?
O1 Ca1 C4 78.0(2) . 7_544 ?
O4 Ca1 C4 82.3(2) 6_554 7_544 ?
O5 Ca1 C4 166.2(3) . 7_544 ?
O2 Ca1 C4 116.31(19) 4_455 7_544 ?
O3 Ca1 C4 89.48(19) 4_454 7_544 ?
O2 Ca1 C4 23.52(18) 7_544 7_544 ?
O3 Ca1 C4 50.46(18) 7_544 7_544 ?
O1 Ca1 C3 78.9(2) . 7_544 ?
O4 Ca1 C3 81.4(2) 6_554 7_544 ?
O5 Ca1 C3 166.1(3) . 7_544 ?
O2 Ca1 C3 89.23(19) 4_455 7_544 ?
O3 Ca1 C3 116.5(2) 4_454 7_544 ?
O2 Ca1 C3 50.61(18) 7_544 7_544 ?
O3 Ca1 C3 23.35(19) 7_544 7_544 ?
C4 Ca1 C3 27.10(17) 7_544 7_544 ?
O1 Ca1 Ca1 79.14(13) . 6 ?
O4 Ca1 Ca1 93.61(13) 6_554 6 ?
O5 Ca1 Ca1 110.8(2) . 6 ?
O2 Ca1 Ca1 34.66(12) 4_455 6 ?
O3 Ca1 Ca1 170.81(14) 4_454 6 ?
O2 Ca1 Ca1 105.45(12) 7_544 6 ?
O3 Ca1 Ca1 32.59(11) 7_544 6 ?
C4 Ca1 Ca1 82.07(14) 7_544 6 ?
C3 Ca1 Ca1 55.32(15) 7_544 6 ?
O1 Ca1 Ca1 94.12(14) . 6_554 ?
O4 Ca1 Ca1 78.26(14) 6_554 6_554 ?
O5 Ca1 Ca1 112.0(2) . 6_554 ?
O2 Ca1 Ca1 168.12(13) 4_455 6_554 ?
O3 Ca1 Ca1 34.95(12) 4_454 6_554 ?
O2 Ca1 Ca1 32.37(11) 7_544 6_554 ?
O3 Ca1 Ca1 104.79(12) 7_544 6_554 ?
C4 Ca1 Ca1 55.30(14) 7_544 6_554 ?
C3 Ca1 Ca1 81.87(15) 7_544 6_554 ?
Ca1 Ca1 Ca1 137.19(6) 6 6_554 ?
O1 Ca1 H18B 85.3 . . ?
O4 Ca1 H18B 114.7 6_554 . ?
O5 Ca1 H18B 17.0 . . ?
O2 Ca1 H18B 87.5 4_455 . ?
O3 Ca1 H18B 68.6 4_454 . ?
O2 Ca1 H18B 130.3 7_544 . ?
O3 Ca1 H18B 149.9 7_544 . ?
C4 Ca1 H18B 151.0 7_544 . ?
C3 Ca1 H18B 163.7 7_544 . ?
Ca1 Ca1 H18B 118.0 6 . ?
Ca1 Ca1 H18B 103.2 6_554 . ?
O1 Ca1 H18A 114.4 . . ?
O4 Ca1 H18A 85.8 6_554 . ?
O5 Ca1 H18A 16.7 . . ?
O2 Ca1 H18A 83.5 4_455 . ?
O3 Ca1 H18A 70.8 4_454 . ?
O2 Ca1 H18A 135.6 7_544 . ?
O3 Ca1 H18A 146.3 7_544 . ?
C4 Ca1 H18A 157.2 7_544 . ?
C3 Ca1 H18A 165.0 7_544 . ?
Ca1 Ca1 H18A 118.2 6 . ?
Ca1 Ca1 H18A 103.2 6_554 . ?
H18B Ca1 H18A 29.3 . . ?
C1 O1 Ca1 143.7(4) . . ?
C4 O2 Ca1 141.1(5) . 12_454 ?
C4 O2 Ca1 102.5(4) . 3 ?
Ca1 O2 Ca1 112.97(19) 12_454 3 ?
C3 O3 Ca1 141.5(5) . 12_455 ?
C3 O3 Ca1 102.4(4) . 3 ?
Ca1 O3 Ca1 112.46(19) 12_455 3 ?
C2 O4 Ca1 144.6(5) . 6 ?
Ca1 O5 H18B 109.9 . . ?
Ca1 O5 H18A 110.1 . . ?
H18B O5 H18A 110.4 . . ?
O1 C1 C2 136.0(7) . . ?
O1 C1 C4 134.9(6) . . ?
C2 C1 C4 89.0(6) . . ?
O4 C2 C3 135.5(7) . . ?
O4 C2 C1 134.6(7) . . ?
C3 C2 C1 89.9(6) . . ?
O3 C3 C4 130.6(7) . . ?
O3 C3 C2 138.8(7) . . ?
C4 C3 C2 90.5(6) . . ?
O3 C3 Ca1 54.2(4) . 3 ?
C4 C3 Ca1 76.4(4) . 3 ?
C2 C3 Ca1 166.9(5) . 3 ?
O2 C4 C3 130.4(7) . . ?
O2 C4 C1 139.0(7) . . ?
C3 C4 C1 90.5(6) . . ?
O2 C4 Ca1 54.0(3) . 3 ?
C3 C4 Ca1 76.5(4) . 3 ?
C1 C4 Ca1 166.9(5) . 3 ?
C7 C6 C5 180.000(16) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
Ca1 O1 C1 C2 7.0(16) . . . . ?
Ca1 O1 C1 C4 -171.1(6) . . . . ?
Ca1 O4 C2 C3 -162.7(6) 6 . . . ?
Ca1 O4 C2 C1 15.5(16) 6 . . . ?
O1 C1 C2 O4 3.7(17) . . . . ?
C4 C1 C2 O4 -177.7(9) . . . . ?
O1 C1 C2 C3 -177.6(9) . . . . ?
C4 C1 C2 C3 1.0(6) . . . . ?
Ca1 O3 C3 C4 155.4(6) 12_455 . . . ?
Ca1 O3 C3 C4 0.6(10) 3 . . . ?
Ca1 O3 C3 C2 -24.4(16) 12_455 . . . ?
Ca1 O3 C3 C2 -179.2(9) 3 . . . ?
Ca1 O3 C3 Ca1 154.8(9) 12_455 . . 3 ?
O4 C2 C3 O3 -2.5(17) . . . . ?
C1 C2 C3 O3 178.8(10) . . . . ?
O4 C2 C3 C4 177.6(9) . . . . ?
C1 C2 C3 C4 -1.1(7) . . . . ?
O4 C2 C3 Ca1 -179.7(17) . . . 3 ?
C1 C2 C3 Ca1 2(3) . . . 3 ?
Ca1 O2 C4 C3 152.9(6) 12_454 . . . ?
Ca1 O2 C4 C3 -3.0(10) 3 . . . ?
Ca1 O2 C4 C1 -25.9(16) 12_454 . . . ?
Ca1 O2 C4 C1 178.2(9) 3 . . . ?
Ca1 O2 C4 Ca1 155.9(8) 12_454 . . 3 ?
O3 C3 C4 O2 1.9(15) . . . . ?
C2 C3 C4 O2 -178.2(8) . . . . ?
Ca1 C3 C4 O2 2.5(8) 3 . . . ?
O3 C3 C4 C1 -178.8(8) . . . . ?
C2 C3 C4 C1 1.1(7) . . . . ?
Ca1 C3 C4 C1 -178.3(5) 3 . . . ?
O3 C3 C4 Ca1 -0.5(8) . . . 3 ?
C2 C3 C4 Ca1 179.4(5) . . . 3 ?
O1 C1 C4 O2 -3.3(17) . . . . ?
C2 C1 C4 O2 178.0(9) . . . . ?
O1 C1 C4 C3 177.6(9) . . . . ?
C2 C1 C4 C3 -1.1(7) . . . . ?
O1 C1 C4 Ca1 170.3(17) . . . 3 ?
C2 C1 C4 Ca1 -8(3) . . . 3 ?
 
_refine_diff_density_max    1.232
_refine_diff_density_min   -0.541
_refine_diff_density_rms    0.124



