 
data_20190820_zju_guo_0m_5_sx
 
_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
 'C11 H4 Ca2 O10' 
_chemical_formula_weight          376.30

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                    20.222(3)
_cell_length_b                    18.433(3)
_cell_length_c                    7.6641(16)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      2856.8(9)
_cell_formula_units_Z             8
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used      5771
_cell_measurement_theta_min        2.99
_cell_measurement_theta_max       32.75
 
_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           0.200
_exptl_crystal_size_mid           0.100
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     0.850
_shelx_estimated_absorpt_T_min    0.848
_shelx_estimated_absorpt_T_max    0.920
_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       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'BRUKER D8 VENTURE PHOTON II'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             6086
_diffrn_reflns_av_unetI/netI      0.0549
_diffrn_reflns_av_R_equivalents   ?
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        26
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        24
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          2.991
_diffrn_reflns_theta_max          28.272
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.971
_diffrn_measured_fraction_theta_full  0.978
_diffrn_reflns_Laue_measured_fraction_max    0.971
_diffrn_reflns_Laue_measured_fraction_full   0.978
_diffrn_reflns_point_group_measured_fraction_max   0.521
_diffrn_reflns_point_group_measured_fraction_full  0.530
_reflns_number_total              6086
_reflns_number_gt                 5438
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      0.000
_reflns_Friedel_fraction_full     0.000
 
_reflns_special_details
;
 _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     ?
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 4-component 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)+(0.0896P)²+11.2336P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack    0.11(4)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          6086
_refine_ls_number_parameters      109
_refine_ls_number_restraints      164
_refine_ls_R_factor_all           0.0704
_refine_ls_R_factor_gt            0.0597
_refine_ls_wR_factor_ref          0.1705
_refine_ls_wR_factor_gt           0.1587
_refine_ls_goodness_of_fit_ref    1.057
_refine_ls_restrained_S_all       1.050
_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 -0.27573(7) 0.52930(8) 0.7035(2) 0.0154(4) Uani 1 1 d . U . . .
O1 O -0.4424(3) 0.2846(3) 1.1537(7) 0.0219(14) Uani 1 1 d . U . . .
O2 O -0.3400(4) 0.4266(3) 0.7478(8) 0.0259(15) Uani 1 1 d . U . . .
O3 O -0.3162(3) 0.3975(4) 1.1629(7) 0.0267(15) Uani 1 1 d . U . . .
O7 O -0.4592(3) 0.3057(4) 0.7589(7) 0.0223(13) Uani 1 1 d . U . . .
O8 O -0.3561(4) 0.6219(4) 0.7000(11) 0.0410(18) Uani 1 1 d . U . . .
C3 C -0.4105(5) 0.3236(5) 1.0482(11) 0.0174(17) Uani 1 1 d . U . . .
C4 C -0.4187(5) 0.3338(5) 0.8637(12) 0.0196(17) Uani 1 1 d . U . . .
C5 C -0.3648(5) 0.3863(5) 0.8621(11) 0.0185(17) Uani 1 1 d . U . . .
C6 C -0.3559(5) 0.3743(5) 1.0480(11) 0.0189(17) Uani 1 1 d . U . . .
C1S C -0.500000 0.500000 0.956(7) 0.098(9) Uani 1 2 d S TU P . .
C2S C -0.500000 0.500000 1.116(8) 0.126(12) Uani 1 2 d S TU P . .
H2S H -0.500000 0.500000 1.237123 0.151 Uiso 1 2 calc R U P . .
C3S C -0.500000 0.500000 0.766(6) 0.107(10) Uani 1 2 d S TU P . .
H3SA H -0.488881 0.452437 0.724706 0.161 Uiso 0.5 1 d R U P A -1
H3SB H -0.468013 0.534345 0.724707 0.161 Uiso 0.5 1 d R U P A -1
H3SC H -0.543106 0.513217 0.724706 0.161 Uiso 0.5 1 d R U 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 O3 2.318(6) 10_464 ?
Ca1 O2 2.321(6) . ?
Ca1 O8 2.357(6) . ?
Ca1 O1 2.389(6) 3_454 ?
Ca1 O7 2.410(6) 3_455 ?
Ca1 O7 2.548(7) 12_454 ?
Ca1 O1 2.566(6) 12_454 ?
Ca1 C4 3.084(9) 12_454 ?
Ca1 C3 3.090(9) 12_454 ?
Ca1 Ca1 4.1152(13) 10_465 ?
Ca1 Ca1 4.1152(13) 10_464 ?
O1 C3 1.259(11) . ?
O2 C5 1.253(10) . ?
O3 C6 1.266(10) . ?
O7 C4 1.260(11) . ?
C3 C4 1.436(10) . ?
C3 C6 1.447(12) . ?
C4 C5 1.457(12) . ?
C5 C6 1.453(11) . ?
C1S C2S 1.23(6) . ?
C1S C3S 1.45(6) . ?
C2S H2S 0.9300 . ?
C3S H3SA 0.9600 . ?
C3S H3SB 0.9600 . ?
C3S H3SC 0.9600 . ?
 
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
O3 Ca1 O2 160.6(2) 10_464 . ?
O3 Ca1 O8 97.5(3) 10_464 . ?
O2 Ca1 O8 101.9(3) . . ?
O3 Ca1 O1 93.6(2) 10_464 3_454 ?
O2 Ca1 O1 91.3(2) . 3_454 ?
O8 Ca1 O1 76.9(3) . 3_454 ?
O3 Ca1 O7 96.6(2) 10_464 3_455 ?
O2 Ca1 O7 87.3(2) . 3_455 ?
O8 Ca1 O7 77.2(3) . 3_455 ?
O1 Ca1 O7 153.12(19) 3_454 3_455 ?
O3 Ca1 O7 81.7(2) 10_464 12_454 ?
O2 Ca1 O7 83.1(2) . 12_454 ?
O8 Ca1 O7 143.4(2) . 12_454 ?
O1 Ca1 O7 66.70(18) 3_454 12_454 ?
O7 Ca1 O7 139.43(16) 3_455 12_454 ?
O3 Ca1 O1 79.7(2) 10_464 12_454 ?
O2 Ca1 O1 84.6(2) . 12_454 ?
O8 Ca1 O1 142.4(2) . 12_454 ?
O1 Ca1 O1 140.48(15) 3_454 12_454 ?
O7 Ca1 O1 66.11(18) 3_455 12_454 ?
O7 Ca1 O1 73.78(17) 12_454 12_454 ?
O3 Ca1 C4 78.5(3) 10_464 12_454 ?
O2 Ca1 C4 82.8(2) . 12_454 ?
O8 Ca1 C4 166.2(3) . 12_454 ?
O1 Ca1 C4 90.1(2) 3_454 12_454 ?
O7 Ca1 C4 116.2(2) 3_455 12_454 ?
O7 Ca1 C4 23.5(2) 12_454 12_454 ?
O1 Ca1 C4 50.3(2) 12_454 12_454 ?
O3 Ca1 C3 77.5(2) 10_464 12_454 ?
O2 Ca1 C3 83.5(3) . 12_454 ?
O8 Ca1 C3 165.2(3) . 12_454 ?
O1 Ca1 C3 117.0(2) 3_454 12_454 ?
O7 Ca1 C3 89.5(2) 3_455 12_454 ?
O7 Ca1 C3 50.4(2) 12_454 12_454 ?
O1 Ca1 C3 23.4(2) 12_454 12_454 ?
C4 Ca1 C3 26.90(19) 12_454 12_454 ?
O3 Ca1 Ca1 94.32(16) 10_464 10_465 ?
O2 Ca1 Ca1 77.95(17) . 10_465 ?
O8 Ca1 Ca1 112.0(2) . 10_465 ?
O1 Ca1 Ca1 167.13(17) 3_454 10_465 ?
O7 Ca1 Ca1 34.98(16) 3_455 10_465 ?
O7 Ca1 Ca1 104.49(14) 12_454 10_465 ?
O1 Ca1 Ca1 32.49(13) 12_454 10_465 ?
C4 Ca1 Ca1 81.54(18) 12_454 10_465 ?
C3 Ca1 Ca1 55.23(16) 12_454 10_465 ?
O3 Ca1 Ca1 79.91(15) 10_464 10_464 ?
O2 Ca1 Ca1 93.64(16) . 10_464 ?
O8 Ca1 Ca1 110.7(2) . 10_464 ?
O1 Ca1 Ca1 35.24(15) 3_454 10_464 ?
O7 Ca1 Ca1 171.63(17) 3_455 10_464 ?
O7 Ca1 Ca1 32.83(14) 12_454 10_464 ?
O1 Ca1 Ca1 105.67(14) 12_454 10_464 ?
C4 Ca1 Ca1 55.73(18) 12_454 10_464 ?
C3 Ca1 Ca1 82.35(17) 12_454 10_464 ?
Ca1 Ca1 Ca1 137.24(8) 10_465 10_464 ?
C3 O1 Ca1 141.2(5) . 7_445 ?
C3 O1 Ca1 102.4(5) . 4_455 ?
Ca1 O1 Ca1 112.3(2) 7_445 4_455 ?
C5 O2 Ca1 144.0(5) . . ?
C6 O3 Ca1 143.0(5) . 10_465 ?
C4 O7 Ca1 141.7(6) . 7_444 ?
C4 O7 Ca1 102.9(5) . 4_455 ?
Ca1 O7 Ca1 112.2(2) 7_444 4_455 ?
O1 C3 C4 130.5(9) . . ?
O1 C3 C6 139.5(8) . . ?
C4 C3 C6 90.1(8) . . ?
O1 C3 Ca1 54.2(4) . 4_455 ?
C4 C3 Ca1 76.3(6) . 4_455 ?
C6 C3 Ca1 166.3(6) . 4_455 ?
O7 C4 C3 130.4(9) . . ?
O7 C4 C5 139.0(8) . . ?
C3 C4 C5 90.6(8) . . ?
O7 C4 Ca1 53.6(4) . 4_455 ?
C3 C4 Ca1 76.8(6) . 4_455 ?
C5 C4 Ca1 167.4(6) . 4_455 ?
O2 C5 C6 136.6(9) . . ?
O2 C5 C4 134.3(7) . . ?
C6 C5 C4 89.0(7) . . ?
O3 C6 C3 134.6(8) . . ?
O3 C6 C5 135.1(9) . . ?
C3 C6 C5 90.3(7) . . ?
C2S C1S C3S 180.00(4) . . ?
C1S C2S H2S 180.0 . . ?
C1S C3S H3SA 109.5 . . ?
C1S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
C1S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
 
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 C3 C4 -150.8(8) 7_445 . . . ?
Ca1 O1 C3 C4 2.5(13) 4_455 . . . ?
Ca1 O1 C3 C6 28(2) 7_445 . . . ?
Ca1 O1 C3 C6 -178.6(12) 4_455 . . . ?
Ca1 O1 C3 Ca1 -153.3(11) 7_445 . . 4_455 ?
Ca1 O7 C4 C3 -157.3(8) 7_444 . . . ?
Ca1 O7 C4 C3 -1.0(13) 4_455 . . . ?
Ca1 O7 C4 C5 24(2) 7_444 . . . ?
Ca1 O7 C4 C5 -179.8(11) 4_455 . . . ?
Ca1 O7 C4 Ca1 -156.2(11) 7_444 . . 4_455 ?
O1 C3 C4 O7 -1(2) . . . . ?
C6 C3 C4 O7 179.5(10) . . . . ?
Ca1 C3 C4 O7 0.9(11) 4_455 . . . ?
O1 C3 C4 C5 178.0(10) . . . . ?
C6 C3 C4 C5 -1.3(9) . . . . ?
Ca1 C3 C4 C5 -180.0(6) 4_455 . . . ?
O1 C3 C4 Ca1 -2.1(10) . . . 4_455 ?
C6 C3 C4 Ca1 178.6(6) . . . 4_455 ?
Ca1 O2 C5 C6 -15(2) . . . . ?
Ca1 O2 C5 C4 160.4(8) . . . . ?
O7 C4 C5 O2 3(2) . . . . ?
C3 C4 C5 O2 -175.8(11) . . . . ?
Ca1 C4 C5 O2 -176(2) 4_455 . . . ?
O7 C4 C5 C6 -179.6(12) . . . . ?
C3 C4 C5 C6 1.3(9) . . . . ?
Ca1 C4 C5 C6 1(3) 4_455 . . . ?
Ca1 O3 C6 C3 175.9(8) 10_465 . . . ?
Ca1 O3 C6 C5 -3(2) 10_465 . . . ?
O1 C3 C6 O3 3(2) . . . . ?
C4 C3 C6 O3 -177.8(12) . . . . ?
Ca1 C3 C6 O3 -172(2) 4_455 . . . ?
O1 C3 C6 C5 -177.8(12) . . . . ?
C4 C3 C6 C5 1.3(9) . . . . ?
Ca1 C3 C6 C5 7(3) 4_455 . . . ?
O2 C5 C6 O3 -5(2) . . . . ?
C4 C5 C6 O3 177.8(12) . . . . ?
O2 C5 C6 C3 175.7(12) . . . . ?
C4 C5 C6 C3 -1.3(8) . . . . ?
 
_refine_diff_density_max    0.780
_refine_diff_density_min   -0.445
_refine_diff_density_rms    0.103



