# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_barbvan
_database_code_depnum_ccdc_archive 'CCDC 1818969'
_audit_update_record             
;
2018-01-23 deposited with the CCDC.
2018-10-30 downloaded from the CCDC.
;

_chemical_formula_weight         280.24
_chemical_formula_moiety         'C8 H8 O3, C4 H4 N2 O3 '
_cell_formula_units_Z            4
_chemical_formula_sum            'C12 H12 N2 O6'

_cell_length_a                   10.53644(31)
_cell_length_b                   18.23475(57)
_cell_length_c                   6.97824(15)
_cell_angle_alpha                90
_cell_angle_beta                 111.6043(22)
_cell_angle_gamma                90
_cell_volume                     1246.537(63)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'x, y, z'

_diffrn_measurement_device_type  
;
Laboratory Aeris Panalytical powder diffractometer.
;


_diffrn_ambient_temperature      295
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_exptl_crystal_density_diffrn    1.493
_refine_ls_hydrogen_treatment    refall
_refine_ls_shift/su_max          <0.01
_refine_ls_number_parameters     136
_pd_proc_ls_prof_R_factor        0.023
_pd_proc_ls_prof_wR_factor       0.031
_refine_ls_R_Fsqd_factor         0.01
_refine_ls_goodness_of_fit_all   1.91
_cell_measurement_temperature    295
_exptl_crystal_colour            yellow

_computing_cell_refinement       Topas
_computing_structure_solution    Topas
_computing_structure_refinement  Topas

_refine_special_details          
;
The cocrystal of barbituric acid and vanillin was observed as an intermediate
in a solid-state mechanochemical Knoevenagel condensation.
The structure model was refined using restraints on bond distances and angles 
as well as planarity restraints. 
;


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
O1 O 4 0.79339(23) -0.21703(12) 0.78231(29) 1 7.338(51)
O2 O 4 0.71581(24) -0.102755(89) 0.18852(24) 1 7.338(51)
O3 O 4 0.64889(26) 0.01662(13) 0.73543(28) 1 7.338(51)
N1 N 4 0.71987(14) -0.096354(50) 0.75741(12) 1 7.338(51)
N2 N 4 0.75496(16) -0.157029(46) 0.48377(14) 1 7.338(51)
C1 C 4 0.75684(17) -0.160539(58) 0.67751(13) 1 7.338(51)
C2 C 4 0.72130(14) -0.098652(55) 0.36008(12) 1 7.338(51)
C3 C 4 0.690596(91) -0.030456(49) 0.44554(12) 1 7.338(51)
C4 C 4 0.68580(17) -0.033493(60) 0.65733(16) 1 7.338(51)
H1 H 4 0.72216(42) -0.09774(23) 0.87977(54) 1 7.338(51)
H2 H 4 0.77737(42) -0.19677(19) 0.43107(84) 1 7.338(51)
H3 H 4 0.60327(36) -0.01142(22) 0.35335(44) 1 7.338(51)
H4 H 4 0.74348(39) 0.01150(20) 0.43108(52) 1 7.338(51)
C11 C 4 0.778511(89) 0.159990(51) 0.14273(16) 1 7.338(51)
C12 C 4 0.84297(11) 0.228427(47) 0.18532(34) 1 7.338(51)
C13 C 4 0.768485(84) 0.290085(55) 0.16341(47) 1 7.338(51)
C14 C 4 0.629360(87) 0.285498(51) 0.10016(41) 1 7.338(51)
C15 C 4 0.56788(11) 0.218534(47) 0.06422(33) 1 7.338(51)
C16 C 4 0.642366(81) 0.156725(49) 0.08662(29) 1 7.338(51)
C17 C 4 0.85836(11) 0.090757(55) 0.17672(15) 1 7.338(51)
C18 C 4 0.960009(89) 0.367038(54) 0.24875(13) 1 7.338(51)
O11 O 4 0.98120(18) 0.084886(87) 0.22852(14) 1 7.338(51)
O12 O 4 0.81727(13) 0.359774(68) 0.18141(30) 1 7.338(51)
O13 O 4 0.54824(11) 0.346100(90) 0.06987(43) 1 7.338(51)
H12 H 4 0.94303(34) 0.23210(25) 0.22945(88) 1 7.338(51)
H15 H 4 0.47138(36) 0.21813(23) 0.02048(78) 1 7.338(51)
H16 H 4 0.60243(37) 0.10910(22) 0.06029(69) 1 7.338(51)
H17 H 4 0.80320(39) 0.04444(21) 0.15449(61) 1 7.338(51)
H18 H 4 0.99581(40) 0.34500(22) 0.14755(58) 1 7.338(51)
H19 H 4 1.00798(44) 0.34043(22) 0.38285(58) 1 7.338(51)
H20 H 4 0.97762(41) 0.41725(19) 0.25846(59) 1 7.338(51)
H13 H 4 0.59396(33) 0.38966(22) 0.1084(17) 1 7.338(51)

_vrf_GEOM001_barbvan             
;
PROBLEM: _geom_bond_atom_site_label_1 is missing
RESPONSE: can be calculated from atomic coordinates.
;
_vrf_GEOM003_barbvan             
;
PROBLEM: _geom_bond_distance is missing
RESPONSE: can be calculated from atomic coordinates.
;
_vrf_GEOM006_barbvan             
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: can be calculated from atomic coordinates.
;
_vrf_GEOM007_barbvan             
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: can be calculated from atomic coordinates.
;


loop_
_pd_meas_2theta_corrected
_pd_meas_intensity_total
_pd_calc_intensity_total
6.0032 8230 8072.9
6.0086 7983 8066.5
6.0140 8148 8060.0
6.0195 8136 8053.6
6.0249 8137 8047.2
6.0303 8038 8040.8
6.0358 8099 8034.4
6.0412 8038 8028.0
6.0466 8014 8021.7
6.0521 8066 8015.4
6.0575 8056 8009.0
6.0629 8070 8002.7
6.0684 8211 7996.4
6.0738 8163 7990.2
6.0792 8076 7983.9
6.0847 8106 7977.7
6.0901 8163 7971.4
6.0955 7970 7965.2
6.1010 8048 7959.0
6.1064 8011 7952.8
6.1118 8056 7946.7
6.1173 8117 7940.5
6.1227 7852 7934.4
6.1281 7917 7928.2
6.1336 7956 7922.1
6.1390 8053 7916.0
6.1444 8103 7909.9
6.1499 7887 7903.9
6.1553 8025 7897.8
6.1607 8008 7891.8
6.1662 8018 7885.7
6.1716 8008 7879.7
6.1770 7879 7873.7
6.1825 7983 7867.7
6.1879 7855 7861.8
6.1933 7849 7855.8
6.1988 7888 7849.9
6.2042 7924 7843.9
6.2096 7861 7838.0
6.2151 7837 7832.1
6.2205 7788 7826.2
6.2259 7945 7820.4
6.2314 7787 7814.5
6.2368 7828 7808.6
6.2422 7935 7802.8
6.2477 7774 7797.0
6.2531 7845 7791.2
6.2585 7785 7785.4
6.2640 7765 7779.6
6.2694 7759 7773.9
6.2748 7861 7768.1
6.2803 7912 7762.4
6.2857 7829 7756.6
6.2911 7704 7750.9
6.2966 7774 7745.2
6.3020 7622 7739.5
6.3074 7820 7733.9
6.3129 7818 7728.2
6.3183 7800 7722.6
6.3237 7806 7716.9
6.3292 7795 7711.3
6.3346 7654 7705.7
6.3400 7865 7700.1
6.3455 7740 7694.5
6.3509 7683 7689.0
6.3563 7498 7683.4
6.3618 7493 7677.9
6.3672 7818 7672.4
6.3726 7540 7666.8
6.3781 7528 7661.3
6.3835 7628 7655.9
6.3889 7546 7650.4
6.3944 7707 7644.9
6.3998 7644 7639.5
6.4052 7702 7634.0
6.4107 7620 7628.6
6.4161 7617 7623.2
6.4215 7669 7617.8
6.4269 7659 7612.4
6.4324 7663 7607.0
6.4378 7623 7601.7
6.4432 7552 7596.3
6.4487 7535 7591.0
6.4541 7564 7585.7
6.4595 7422 7580.3
6.4650 7501 7575.0
6.4704 7656 7569.8
6.4758 7528 7564.5
6.4813 7468 7559.2
6.4867 7515 7554.0
6.4921 7605 7548.7
6.4976 7554 7543.5
6.5030 7533 7538.3
6.5084 7699 7533.1
6.5139 7463 7527.9
6.5193 7487 7522.7
6.5247 7336 7517.6
6.5302 7409 7512.4
6.5356 7420 7507.3
6.5410 7445 7502.1
6.5465 7444 7497.0
6.5519 7623 7491.9
6.5573 7574 7486.8
6.5628 7393 7481.7
6.5682 7397 7476.7
6.5736 7404 7471.6
6.5791 7368 7466.6
6.5845 7623 7461.5
6.5899 7531 7456.5
6.5954 7421 7451.5
6.6008 7416 7446.5
6.6062 7510 7441.5
6.6117 7444 7436.5
6.6171 7502 7431.6
6.6225 7357 7426.6
6.6280 7329 7421.7
6.6334 7333 7416.7
6.6388 7393 7411.8
6.6443 7250 7406.9
6.6497 7113 7402.0
6.6551 7276 7397.1
6.6606 7387 7392.2
6.6660 7672 7387.4
6.6714 7142 7382.5
6.6769 7421 7377.7
6.6823 7312 7372.8
6.6877 7157 7368.0
6.6932 7343 7363.2
6.6986 7184 7358.4
6.7040 7359 7353.6
6.7095 7161 7348.9
6.7149 7356 7344.1
6.7203 7497 7339.3
6.7258 7201 7334.6
6.7312 7208 7329.9
6.7366 7266 7325.1
6.7421 7329 7320.4
6.7475 7333 7315.7
6.7529 7254 7311.0
6.7584 7281 7306.4
6.7638 7405 7301.7
6.7692 7377 7297.0
6.7747 7134 7292.4
6.7801 7359 7287.8
6.7855 7264 7283.1
6.7910 7288 7278.5
6.7964 7219 7273.9
6.8018 6935 7269.3
6.8073 7190 7264.8
6.8127 7182 7260.2
6.8181 7222 7255.6
6.8236 7283 7251.1
6.8290 7175 7246.5
6.8344 7293 7242.0
6.8399 7350 7237.5
6.8453 7046 7233.0
6.8507 7139 7228.5
6.8562 7375 7224.0
6.8616 7210 7219.5
6.8670 7158 7215.0
6.8725 7201 7210.6
6.8779 7137 7206.1
6.8833 7221 7201.7
6.8888 7226 7197.3
6.8942 7143 7192.8
6.8996 7192 7188.4
6.9051 7116 7184.0
6.9105 7085 7179.6
6.9159 6984 7175.3
6.9214 7106 7170.9
6.9268 7168 7166.5
6.9322 6962 7162.2
6.9377 7227 7157.9
6.9431 7199 7153.5
6.9485 7089 7149.2
6.9540 7015 7144.9
6.9594 7047 7140.6
6.9648 7058 7136.3
6.9703 7133 7132.0
6.9757 7170 7127.8
6.9811 7232 7123.5
6.9866 7191 7119.2
6.9920 7079 7115.0
6.9974 7229 7110.8
7.0029 7114 7106.6
7.0083 7155 7102.3
7.0137 7014 7098.1
7.0192 6958 7093.9
7.0246 6956 7089.8
7.0300 7052 7085.6
7.0355 7047 7081.4
7.0409 7044 7077.3
7.0463 7119 7073.1
7.0518 7068 7069.0
7.0572 7104 7064.9
7.0626 7029 7060.8
7.0681 7077 7056.6
7.0735 6864 7052.5
7.0789 7107 7048.5
7.0844 7067 7044.4
7.0898 6940 7040.3
7.0952 6917 7036.2
7.1007 7038 7032.2
7.1061 7096 7028.2
7.1115 6965 7024.1
7.1170 7048 7020.1
7.1224 7293 7016.1
7.1278 7078 7012.1
7.1333 6834 7008.1
7.1387 7068 7004.1
7.1441 7106 7000.1
7.1496 6967 6996.1
7.1550 6882 6992.2
7.1604 7012 6988.2
7.1659 7052 6984.3
7.1713 6897 6980.4
7.1767 6830 6976.4
7.1822 7007 6972.5
7.1876 6990 6968.6
7.1930 6813 6964.7
7.1985 6843 6960.8
7.2039 6918 6957.0
7.2093 6886 6953.1
7.2148 6924 6949.2
7.2202 7052 6945.4
7.2256 6966 6941.5
7.2311 6823 6937.7
7.2365 7024 6933.9
7.2419 7121 6930.1
7.2474 6928 6926.3
7.2528 6786 6922.5
7.2582 7014 6918.7
7.2637 6787 6914.9
7.2691 6959 6911.1
7.2745 6943 6907.4
7.2800 6901 6903.6
7.2854 6884 6899.9
7.2908 7080 6896.1
7.2963 6973 6892.4
7.3017 6824 6888.7
7.3071 6883 6885.0
7.3126 6823 6881.3
7.3180 7003 6877.6
7.3234 6940 6873.9
7.3289 6910 6870.2
7.3343 6799 6866.6
7.3397 6749 6862.9
7.3452 6787 6859.3
7.3506 6825 6855.6
7.3560 6884 6852.0
7.3615 6789 6848.4
7.3669 6740 6844.8
7.3723 7008 6841.2
7.3778 6881 6837.6
7.3832 6902 6834.0
7.3886 6802 6830.4
7.3941 6768 6826.9
7.3995 6655 6823.3
7.4049 6796 6819.8
7.4104 6817 6816.3
7.4158 6579 6812.7
7.4212 6871 6809.2
7.4267 6615 6805.8
7.4321 6838 6802.3
7.4375 6788 6798.8
7.4430 6735 6795.4
7.4484 6661 6792.0
7.4538 6762 6788.7
7.4593 6792 6785.5
7.4647 6787 6782.0
7.4701 6745 6778.6
7.4756 6678 6775.1
7.4810 6629 6771.7
7.4864 6758 6768.2
7.4919 6798 6764.8
7.4973 6683 6761.3
7.5027 6671 6757.9
7.5082 6647 6754.5
7.5136 6674 6751.1
7.5190 6623 6747.7
7.5245 6664 6744.3
7.5299 6553 6740.9
7.5353 6780 6737.6
7.5408 6685 6734.2
7.5462 6718 6730.9
7.5516 6851 6727.5
7.5571 6758 6724.2
7.5625 6667 6720.8
7.5679 6838 6717.5
7.5734 6766 6714.2
7.5788 6665 6710.9
7.5842 6827 6707.6
7.5897 6611 6704.3
7.5951 6664 6701.1
7.6005 6541 6697.8
7.6060 6748 6694.5
7.6114 6564 6691.3
7.6168 6618 6688.0
7.6223 6607 6684.8
7.6277 6589 6681.6
7.6331 6844 6678.4
7.6386 6657 6675.2
7.6440 6658 6672.0
7.6494 6608 6668.8
7.6549 6730 6665.6
7.6603 6647 6662.5
7.6657 6538 6659.3
7.6712 6661 6656.1
7.6766 6505 6653.0
7.6820 6594 6649.9
7.6875 6472 6646.8
7.6929 6567 6643.7
7.6983 6608 6640.6
7.7038 6582 6637.5
7.7092 6628 6634.4
7.7146 6659 6631.3
7.7201 6605 6628.3
7.7255 6742 6625.2
7.7309 6634 6622.2
7.7364 6652 6619.1
7.7418 6652 6616.1
7.7472 6621 6613.1
7.7527 6598 6610.1
7.7581 6662 6607.2
7.7635 6546 6604.2
7.7690 6568 6601.2
7.7744 6559 6598.3
7.7798 6730 6595.3
7.7853 6516 6592.4
7.7907 6627 6589.5
7.7961 6541 6586.6
7.8016 6487 6583.7
7.8070 6569 6580.9
7.8124 6440 6578.0
7.8179 6637 6575.2
7.8233 6575 6572.4
7.8287 6491 6569.6
7.8342 6561 6566.8
7.8396 6422 6564.0
7.8450 6534 6561.3
7.8505 6443 6558.6
7.8559 6608 6555.9
7.8613 6509 6553.2
7.8668 6387 6550.5
7.8722 6483 6547.9
7.8776 6487 6545.3
7.8831 6684 6542.8
7.8885 6471 6540.3
7.8939 6365 6537.9
7.8994 6507 6535.7
7.9048 6518 6533.6
7.9102 6458 6531.5
7.9157 6535 6529.8
7.9211 6417 6527.7
7.9265 6402 6525.0
7.9320 6523 6522.2
7.9374 6419 6519.4
7.9428 6380 6516.7
7.9483 6436 6514.0
7.9537 6558 6511.3
7.9591 6457 6508.5
7.9646 6470 6505.8
7.9700 6587 6503.2
7.9754 6503 6500.5
7.9809 6420 6497.8
7.9863 6368 6495.2
7.9917 6494 6492.5
7.9972 6542 6489.9
8.0026 6391 6487.3
8.0080 6537 6484.6
8.0135 6406 6482.0
8.0189 6447 6479.5
8.0243 6579 6476.9
8.0297 6492 6474.3
8.0352 6550 6471.8
8.0406 6574 6469.3
8.0460 6456 6466.8
8.0515 6406 6464.3
8.0569 6488 6461.9
8.0623 6420 6459.4
8.0678 6487 6457.1
8.0732 6407 6454.9
8.0786 6402 6452.7
8.0841 6394 6450.2
8.0895 6510 6447.7
8.0949 6374 6445.2
8.1004 6549 6442.7
8.1058 6456 6440.2
8.1112 6526 6437.7
8.1167 6395 6435.3
8.1221 6458 6432.9
8.1275 6339 6430.4
8.1330 6564 6428.0
8.1384 6457 6425.6
8.1438 6577 6423.2
8.1493 6517 6420.8
8.1547 6480 6418.4
8.1601 6494 6416.1
8.1656 6460 6413.7
8.1710 6362 6411.4
8.1764 6419 6409.1
8.1819 6477 6406.8
8.1873 6323 6404.5
8.1927 6366 6402.2
8.1982 6412 6399.9
8.2036 6259 6397.7
8.2090 6449 6395.4
8.2145 6461 6393.2
8.2199 6498 6391.0
8.2253 6369 6388.8
8.2308 6492 6386.6
8.2362 6439 6384.4
8.2416 6431 6382.3
8.2471 6286 6380.2
8.2525 6347 6378.1
8.2579 6404 6376.0
8.2634 6411 6373.9
8.2688 6464 6371.9
8.2742 6166 6369.8
8.2797 6292 6367.8
8.2851 6402 6365.9
8.2905 6317 6363.9
8.2960 6279 6362.0
8.3014 6304 6360.1
8.3068 6456 6358.2
8.3123 6296 6356.4
8.3177 6217 6354.6
8.3231 6332 6352.8
8.3286 6425 6351.1
8.3340 6314 6349.4
8.3394 6503 6347.7
8.3449 6542 6346.2
8.3503 6248 6344.6
8.3557 6357 6343.1
8.3612 6344 6341.7
8.3666 6248 6340.4
8.3720 6366 6339.1
8.3775 6416 6337.9
8.3829 6305 6336.9
8.3883 6315 6335.9
8.3938 6191 6335.0
8.3992 6381 6334.2
8.4046 6475 6333.7
8.4101 6307 6333.3
8.4155 6277 6333.2
8.4209 6331 6333.6
8.4264 6318 6333.8
8.4318 6396 6333.5
8.4372 6415 6333.2
8.4427 6433 6333.2
8.4481 6409 6333.2
8.4535 6387 6333.5
8.4590 6299 6333.9
8.4644 6372 6334.5
8.4698 6355 6335.3
8.4753 6408 6336.3
8.4807 6343 6337.5
8.4861 6476 6338.9
8.4916 6309 6340.5
8.4970 6235 6342.4
8.5024 6403 6344.5
8.5079 6246 6346.9
8.5133 6328 6349.4
8.5187 6420 6352.3
8.5242 6353 6355.3
8.5296 6506 6358.7
8.5350 6354 6362.3
8.5405 6398 6366.1
8.5459 6383 6370.2
8.5513 6416 6374.6
8.5568 6603 6379.3
8.5622 6481 6384.2
8.5676 6338 6389.4
8.5731 6426 6394.9
8.5785 6538 6400.6
8.5839 6312 6406.6
8.5894 6342 6412.9
8.5948 6262 6419.4
8.6002 6492 6426.2
8.6057 6389 6433.3
8.6111 6587 6440.7
8.6165 6620 6448.3
8.6220 6469 6456.3
8.6274 6402 6464.5
8.6328 6410 6473.0
8.6383 6605 6481.9
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34.7069 1933 2040.5
34.7123 2003 2040.3
34.7177 2022 2039.9
34.7232 1989 2039.4
34.7286 1974 2038.8
34.7340 1972 2038.0
34.7395 2061 2037.2
34.7449 1984 2036.3
34.7503 1929 2035.2
34.7558 2013 2033.9
34.7612 2059 2032.5
34.7666 1897 2030.8
34.7721 1912 2029.0
34.7775 1896 2027.0
34.7829 1939 2024.8
34.7884 1901 2022.5
34.7938 1980 2020.1
34.7992 1853 2017.6
34.8047 1860 2014.9
34.8101 1902 2012.0
34.8155 1909 2009.1
34.8210 1956 2006.1
34.8264 1936 2002.9
34.8318 1888 1999.7
34.8373 1807 1996.4
34.8427 1864 1993.1
34.8481 1860 1989.7
34.8536 1892 1986.4
34.8590 1962 1983.0
34.8644 1942 1979.7
34.8699 1912 1976.3
34.8753 1888 1973.1
34.8807 1901 1969.9
34.8862 1907 1966.7
34.8916 1888 1963.7
34.8970 1928 1960.7
34.9025 1898 1957.9
34.9079 1938 1955.2
34.9133 1899 1952.6
34.9188 1854 1950.1
34.9242 1856 1947.7
34.9296 1943 1945.6
34.9351 1914 1943.5
34.9405 1873 1941.6
34.9459 1926 1940.2
34.9514 1896 1939.0
34.9568 1962 1938.0
34.9622 1847 1937.2
34.9677 1913 1936.7
34.9731 1878 1936.3
34.9785 1854 1936.3
34.9840 1936 1936.4
34.9894 1945 1936.8
34.9948 1893 1937.5
35.0003 1972 1938.4
35.0057 1952 1939.6
35.0111 1908 1941.0
35.0166 1938 1942.7
35.0220 1977 1944.6
35.0274 1902 1946.7
35.0329 1954 1949.2
35.0383 1957 1951.8
35.0437 1975 1954.7
35.0492 1874 1957.8
35.0546 1984 1961.2
35.0600 1994 1964.8
35.0655 1825 1968.7
35.0709 1964 1972.7
35.0763 2009 1977.0
35.0818 2010 1981.5
35.0872 1985 1986.2
35.0926 1941 1991.0
35.0981 2020 1996.0
35.1035 1947 2001.2
35.1089 2015 2006.5
35.1144 2053 2011.9
35.1198 1989 2017.5
35.1252 2065 2023.1
35.1307 2036 2028.8
35.1361 2026 2034.5
35.1415 2100 2040.3
35.1470 2056 2046.2
35.1524 2091 2052.0
35.1578 2081 2057.8
35.1633 2108 2063.6
35.1687 2059 2069.3
35.1741 1990 2075.0
35.1796 2066 2080.7
35.1850 2131 2086.3
35.1904 2098 2091.8
35.1958 2116 2097.3
35.2013 2218 2102.6
35.2067 2159 2107.9
35.2121 2189 2113.1
35.2176 2165 2118.3
35.2230 2187 2123.5
35.2284 2129 2128.6
35.2339 2163 2133.8
35.2393 2205 2138.9
35.2447 2140 2144.1
35.2502 2130 2149.3
35.2556 2267 2154.5
35.2610 2192 2159.9
35.2665 2219 2165.5
35.2719 2296 2171.2
35.2773 2276 2177.1
35.2828 2230 2183.1
35.2882 2192 2189.3
35.2936 2252 2195.7
35.2991 2248 2202.2
35.3045 2199 2209.0
35.3099 2160 2215.9
35.3154 2235 2223.2
35.3208 2316 2230.8
35.3262 2221 2238.5
35.3317 2233 2246.6
35.3371 2288 2254.9
35.3425 2247 2263.4
35.3480 2250 2272.2
35.3534 2185 2281.2
35.3588 2200 2290.5
35.3643 2271 2300.0
35.3697 2251 2309.7
35.3751 2309 2319.5
35.3806 2296 2329.6
35.3860 2334 2339.7
35.3914 2265 2350.0
35.3969 2368 2360.4
35.4023 2374 2370.8
35.4077 2270 2381.4
35.4132 2341 2391.9
35.4186 2263 2402.5
35.4240 2351 2413.1
35.4295 2380 2423.6
35.4349 2320 2434.1
35.4403 2399 2444.6
35.4458 2451 2455.0
35.4512 2412 2465.3
35.4566 2396 2475.6
35.4621 2435 2485.7
35.4675 2388 2495.6
35.4729 2477 2505.5
35.4784 2413 2515.3
35.4838 2475 2525.1
35.4892 2567 2534.7
35.4947 2469 2544.2
35.5001 2433 2553.7
35.5055 2536 2563.0
35.5110 2544 2572.2
35.5164 2504 2581.3
35.5218 2533 2590.3
35.5273 2530 2599.1
35.5327 2570 2607.7
35.5381 2541 2616.0
35.5436 2505 2624.1
35.5490 2622 2632.0
35.5544 2592 2639.5
35.5599 2630 2646.7
35.5653 2658 2653.5
35.5707 2638 2659.9
35.5762 2774 2665.8
35.5816 2719 2671.2
35.5870 2675 2676.0
35.5925 2648 2680.2
35.5979 2728 2683.8
35.6033 2577 2686.7
35.6088 2714 2688.9
35.6142 2753 2690.3
35.6196 2736 2691.1
35.6251 2643 2691.1
35.6305 2767 2690.3
35.6359 2556 2688.7
35.6414 2731 2686.3
35.6468 2612 2683.0
35.6522 2656 2678.8
35.6577 2689 2673.8
35.6631 2716 2667.9
35.6685 2631 2661.3
35.6740 2672 2653.8
35.6794 2643 2645.5
35.6848 2592 2636.4
35.6903 2632 2626.6
35.6957 2621 2616.0
35.7011 2629 2604.8
35.7066 2587 2592.9
35.7120 2647 2580.3
35.7174 2492 2567.2
35.7229 2569 2553.6
35.7283 2585 2539.4
35.7337 2474 2524.8
35.7392 2469 2509.8
35.7446 2490 2494.4
35.7500 2412 2478.8
35.7555 2505 2463.0
35.7609 2427 2446.9
35.7663 2447 2430.6
35.7718 2367 2414.2
35.7772 2323 2397.7
35.7826 2386 2381.1
35.7881 2377 2364.5
35.7935 2472 2348.2
35.7989 2316 2332.0
35.8044 2289 2315.9
35.8098 2294 2300.0
35.8152 2215 2284.3
35.8207 2226 2268.8
35.8261 2181 2253.6
35.8315 2141 2238.7
35.8370 2175 2224.0
35.8424 2164 2209.7
35.8478 2205 2195.8
35.8533 2147 2182.2
35.8587 2073 2168.9
35.8641 2092 2156.0
35.8696 2126 2143.5
35.8750 2088 2131.4
35.8804 2113 2119.7
35.8859 2055 2108.4
35.8913 1967 2097.5
35.8967 2024 2087.0
35.9022 2032 2077.0
35.9076 2014 2067.3
35.9130 2009 2058.1
35.9185 1973 2049.3
35.9239 2062 2040.9
35.9293 2062 2032.8
35.9348 2012 2025.2
35.9402 1910 2018.1
35.9456 2052 2011.3
35.9511 2022 2004.9
35.9565 2006 1998.8
35.9619 2017 1993.2
35.9674 2075 1988.0
35.9728 2063 1983.1
35.9782 1995 1978.6
35.9837 2002 1974.4
35.9891 1934 1970.7
35.9945 2033 1967.2
36.0000 1898 1964.1
36.0054 2020 1961.3
36.0108 1984 1959.0
36.0163 1882 1957.0
36.0217 1970 1955.5
36.0271 1949 1954.3
36.0326 1914 1953.4
36.0380 1913 1953.0
36.0434 1947 1952.9
36.0489 1953 1953.1
36.0543 1911 1953.7
36.0597 1964 1954.7
36.0652 1991 1956.0
36.0706 1959 1957.7
36.0760 1954 1959.8
36.0815 2036 1962.3
36.0869 1947 1965.2
36.0923 1946 1968.5
36.0978 1969 1972.1
36.1032 1910 1976.1
36.1086 1897 1980.6
36.1141 2068 1985.4
36.1195 2022 1990.7
36.1249 2043 1996.3
36.1304 2114 2002.3
36.1358 2096 2008.7
36.1412 2096 2015.6
36.1467 2015 2022.8
36.1521 2047 2030.6
36.1575 2070 2038.8
36.1630 2136 2047.5
36.1684 2160 2056.5
36.1738 2222 2066.0
36.1793 2164 2075.8
36.1847 2134 2086.1
36.1901 2090 2096.8
36.1956 2206 2107.8
36.2010 2126 2119.2
36.2064 2189 2131.0
36.2119 2154 2143.1
36.2173 2242 2155.6
36.2227 2214 2168.3
36.2282 2241 2181.4
36.2336 2381 2194.6
36.2390 2377 2208.1
36.2445 2268 2221.8
36.2499 2246 2235.6
36.2553 2235 2249.6
36.2608 2410 2263.7
36.2662 2301 2277.8
36.2716 2415 2291.9
36.2771 2377 2305.9
36.2825 2424 2319.8
36.2879 2326 2333.7
36.2934 2412 2347.3
36.2988 2429 2360.7
36.3042 2373 2373.8
36.3097 2454 2386.7
36.3151 2464 2399.2
36.3205 2477 2411.4
36.3260 2510 2423.1
36.3314 2474 2434.5
36.3368 2406 2445.4
36.3423 2516 2455.9
36.3477 2583 2466.1
36.3531 2575 2475.7
36.3586 2497 2484.9
36.3640 2605 2493.8
36.3694 2488 2502.2
36.3749 2685 2510.2
36.3803 2564 2517.9
36.3857 2540 2525.3
36.3912 2566 2532.4
36.3966 2612 2539.2
36.4020 2567 2545.8
36.4075 2551 2552.1
36.4129 2610 2558.3
36.4183 2556 2564.3
36.4238 2699 2570.2
36.4292 2557 2576.0
36.4346 2654 2581.8
36.4401 2572 2587.6
36.4455 2656 2593.4
36.4509 2624 2599.3
36.4564 2542 2605.3
36.4618 2572 2611.3
36.4672 2580 2617.5
36.4727 2559 2623.9
36.4781 2680 2630.4
36.4835 2655 2637.2
36.4890 2585 2644.1
36.4944 2655 2651.3
36.4998 2640 2658.8
36.5053 2745 2666.5
36.5107 2699 2674.4
36.5161 2705 2682.7
36.5216 2544 2691.1
36.5270 2719 2699.8
36.5324 2661 2708.8
36.5379 2670 2718.0
36.5433 2723 2727.3
36.5487 2711 2737.0
36.5542 2800 2746.8
36.5596 2814 2756.7
36.5650 2816 2766.8
36.5705 2830 2776.9
36.5759 2821 2787.1
36.5813 2785 2797.3
36.5868 2844 2807.5
36.5922 2817 2817.5
36.5976 2833 2827.4
36.6031 2820 2837.0
36.6085 2820 2846.4
36.6139 2954 2855.4
36.6194 2854 2863.9
36.6248 2817 2872.0
36.6302 2734 2879.6
36.6357 2844 2886.5
36.6411 2952 2892.8
36.6465 2925 2898.3
36.6520 2898 2902.9
36.6574 2925 2906.7
36.6628 2821 2909.7
36.6683 3001 2911.9
36.6737 2853 2913.2
36.6791 2936 2913.9
36.6846 2967 2913.8
36.6900 2949 2913.0
36.6954 2914 2911.4
36.7009 2987 2909.2
36.7063 2893 2906.5
36.7117 2873 2903.2
36.7172 2943 2899.4
36.7226 2949 2895.2
36.7280 2926 2890.7
36.7335 2923 2886.0
36.7389 2910 2881.1
36.7443 2831 2876.1
36.7498 2919 2871.1
36.7552 2831 2866.1
36.7606 2853 2861.4
36.7661 3005 2856.8
36.7715 2873 2852.6
36.7769 2895 2848.8
36.7823 2803 2845.6
36.7878 2808 2843.0
36.7932 2790 2841.1
36.7986 2847 2840.0
36.8041 2784 2839.8
36.8095 2750 2840.5
36.8149 2770 2842.2
36.8204 2870 2845.0
36.8258 2800 2849.1
36.8312 2860 2854.4
36.8367 2843 2861.0
36.8421 2887 2869.1
36.8475 2846 2878.6
36.8530 2825 2889.6
36.8584 2873 2902.1
36.8638 2902 2916.1
36.8693 2884 2931.6
36.8747 2968 2948.7
36.8801 2942 2967.4
36.8856 3090 2987.6
36.8910 2994 3009.3
36.8964 3060 3032.5
36.9019 2953 3057.2
36.9073 3153 3083.2
36.9127 3115 3110.6
36.9182 3180 3139.2
36.9236 3259 3169.1
36.9290 3442 3200.0
36.9345 3207 3232.0
36.9399 3324 3264.8
36.9453 3359 3298.4
36.9508 3414 3332.7
36.9562 3407 3367.6
36.9616 3492 3403.0
36.9671 3558 3438.7
36.9725 3617 3474.6
36.9779 3676 3510.6
36.9834 3688 3546.5
36.9888 3590 3582.3
36.9942 3732 3617.8
36.9997 3763 3653.0
37.0051 3882 3687.7
37.0105 3929 3721.8
37.0160 3941 3755.4
37.0214 3769 3788.2
37.0268 3991 3820.3
37.0323 4065 3851.6
37.0377 4066 3882.0
37.0431 4124 3911.5
37.0486 4078 3940.2
37.0540 4284 3967.9
37.0594 4096 3994.6
37.0649 4137 4020.3
37.0703 4091 4044.8
37.0757 4282 4068.2
37.0812 4183 4090.3
37.0866 4231 4111.1
37.0920 4214 4130.4
37.0975 4309 4148.3
37.1029 4302 4164.5
37.1083 4254 4179.1
37.1138 4414 4191.9
37.1192 4339 4202.8
37.1246 4219 4211.8
37.1301 4335 4218.7
37.1355 4225 4223.5
37.1409 4362 4226.2
37.1464 4091 4226.6
37.1518 4155 4224.7
37.1572 4314 4220.5
37.1627 4236 4214.0
37.1681 4230 4205.0
37.1735 4160 4193.6
37.1790 4085 4179.9
37.1844 4187 4163.9
37.1898 4110 4145.6
37.1953 4114 4125.2
37.2007 4044 4102.5
37.2061 3934 4077.8
37.2116 4004 4051.1
37.2170 3938 4022.6
37.2224 3875 3992.2
37.2279 3863 3959.9
37.2333 3902 3926.0
37.2387 3809 3890.5
37.2442 3760 3853.5
37.2496 3625 3815.2
37.2550 3633 3775.5
37.2605 3689 3734.7
37.2659 3575 3692.8
37.2713 3518 3650.0
37.2768 3429 3606.2
37.2822 3501 3561.8
37.2876 3292 3516.7
37.2931 3177 3471.0
37.2985 3283 3424.9
37.3039 3358 3378.6
37.3094 3251 3332.0
37.3148 3173 3285.4
37.3202 3139 3238.9
37.3257 3004 3192.4
37.3311 3039 3146.3
37.3365 3033 3100.5
37.3420 2958 3055.1
37.3474 2991 3010.3
37.3528 2900 2966.1
37.3583 2808 2922.6
37.3637 2777 2879.9
37.3691 2774 2838.0
37.3746 2696 2796.8
37.3800 2578 2756.4
37.3854 2642 2717.0
37.3909 2668 2678.5
37.3963 2609 2641.1
37.4017 2652 2604.6
37.4072 2461 2569.1
37.4126 2452 2534.7
37.4180 2405 2501.3
37.4235 2485 2469.0
37.4289 2406 2437.7
37.4343 2318 2407.4
37.4398 2342 2378.2
37.4452 2279 2350.0
37.4506 2314 2322.9
37.4561 2167 2296.7
37.4615 2213 2271.5
37.4669 2229 2247.3
37.4724 2149 2224.0
37.4778 2224 2201.7
37.4832 2144 2180.3
37.4887 2186 2159.8
37.4941 2217 2140.1
37.4995 2202 2121.3
37.5050 2053 2103.4
37.5104 2050 2086.2
37.5158 2073 2069.7
37.5213 2020 2054.1
37.5267 2015 2039.1
37.5321 1935 2024.8
37.5376 1968 2011.2
37.5430 2063 1998.2
37.5484 1953 1985.9
37.5539 1966 1974.2
37.5593 1976 1963.1
37.5647 1957 1952.5
37.5702 1952 1942.5
37.5756 1892 1933.0
37.5810 1965 1923.9
37.5865 1976 1915.4
37.5919 1858 1907.3
37.5973 1915 1899.6
37.6028 1824 1892.3
37.6082 1852 1885.5
37.6136 1869 1879.0
37.6191 1889 1873.0
37.6245 1825 1867.2
37.6299 1903 1861.9
37.6354 1871 1856.8
37.6408 1831 1852.1
37.6462 1859 1847.6
37.6517 1799 1843.5
37.6571 1889 1839.7
37.6625 1731 1836.1
37.6680 1811 1832.8
37.6734 1769 1829.8
37.6788 1755 1827.0
37.6843 1810 1824.5
37.6897 1819 1822.2
37.6951 1813 1820.2
37.7006 1884 1818.3
37.7060 1814 1816.7
37.7114 1789 1815.4
37.7169 1840 1814.2
37.7223 1773 1813.3
37.7277 1813 1812.6
37.7332 1834 1812.1
37.7386 1851 1811.8
37.7440 1756 1811.7
37.7495 1789 1811.9
37.7549 1855 1812.2
37.7603 1830 1812.7
37.7658 1766 1813.5
37.7712 1906 1814.4
37.7766 1735 1815.5
37.7821 1802 1816.9
37.7875 1823 1818.5
37.7929 1795 1820.2
37.7984 1805 1822.2
37.8038 1808 1824.4
37.8092 1784 1826.8
37.8147 1824 1829.4
37.8201 1825 1832.3
37.8255 1781 1835.4
37.8310 1854 1838.7
37.8364 1881 1842.2
37.8418 1875 1846.0
37.8473 1835 1850.0
37.8527 1825 1854.3
37.8581 1847 1858.8
37.8636 1803 1863.5
37.8690 1893 1868.6
37.8744 1819 1873.9
37.8799 1825 1879.3
37.8853 1863 1885.0
37.8907 1793 1890.9
37.8962 1842 1897.0
37.9016 1889 1903.4
37.9070 1934 1909.9
37.9125 1987 1916.7
37.9179 1895 1923.7
37.9233 1889 1930.9
37.9288 1916 1938.2
37.9342 1860 1945.7
37.9396 1929 1953.4
37.9451 1983 1961.2
37.9505 1987 1969.0
37.9559 1950 1977.0
37.9614 1915 1985.0
37.9668 1978 1993.1
37.9722 1982 2001.2
37.9777 1974 2009.2
37.9831 2014 2017.2
37.9885 2008 2025.2
37.9940 2000 2033.0
37.9994 1998 2040.6
38.0048 2029 2048.0
38.0103 2056 2055.3
38.0157 2044 2062.2
38.0211 1984 2068.9
38.0266 2016 2075.2
38.0320 2048 2081.2
38.0374 1985 2086.8
38.0429 2086 2091.9
38.0483 2063 2096.6
38.0537 2054 2100.8
38.0592 2062 2104.5
38.0646 2024 2107.6
38.0700 2051 2110.3
38.0755 2042 2112.3
38.0809 2043 2113.9
38.0863 2137 2114.8
38.0918 2047 2115.1
38.0972 2017 2114.9
38.1026 2100 2114.1
38.1081 2041 2112.7
38.1135 2079 2110.7
38.1189 2168 2108.2
38.1244 2085 2105.2
38.1298 2020 2101.7
38.1352 2107 2097.7
38.1407 2064 2093.3
38.1461 2047 2088.4
38.1515 2089 2083.1
38.1570 2172 2077.3
38.1624 1991 2071.3
38.1678 2124 2064.9
38.1733 2093 2058.2
38.1787 2064 2051.2
38.1841 2043 2044.0
38.1896 2030 2036.6
38.1950 1958 2029.0
38.2004 2063 2021.2
38.2059 1993 2013.4
38.2113 2064 2005.4
38.2167 2046 1997.3
38.2222 1936 1989.2
38.2276 1948 1981.2
38.2330 2042 1973.1
38.2385 1880 1965.1
38.2439 1963 1957.3
38.2493 1887 1949.4
38.2548 1968 1941.7
38.2602 1907 1934.1
38.2656 1925 1926.6
38.2711 1963 1919.3
38.2765 1939 1912.3
38.2819 1926 1905.4
38.2874 1899 1898.8
38.2928 1888 1892.5
38.2982 1855 1886.4
38.3037 1868 1880.6
38.3091 1859 1875.1
38.3145 1874 1869.9
38.3200 1855 1865.0
38.3254 1898 1860.4
38.3308 1767 1856.1
38.3363 1803 1852.1
38.3417 1816 1848.5
38.3471 1848 1845.2
38.3526 1805 1842.2
38.3580 1836 1839.5
38.3634 1789 1837.1
38.3689 1812 1835.0
38.3743 1750 1833.2
38.3797 1810 1831.6
38.3851 1790 1830.3
38.3906 1841 1829.2
38.3960 1747 1828.4
38.4014 1815 1827.8
38.4069 1762 1827.3
38.4123 1779 1827.1
38.4177 1714 1826.9
38.4232 1748 1826.9
38.4286 1765 1826.9
38.4340 1781 1827.0
38.4395 1678 1827.2
38.4449 1800 1827.3
38.4503 1689 1827.4
38.4558 1702 1827.4
38.4612 1787 1827.4
38.4666 1792 1827.2
38.4721 1793 1826.9
38.4775 1667 1826.4
38.4829 1733 1825.9
38.4884 1778 1825.1
38.4938 1672 1824.2
38.4992 1737 1823.1
38.5047 1689 1821.8
38.5101 1778 1820.4
38.5155 1763 1818.8
38.5210 1662 1817.1
38.5264 1746 1815.2
38.5318 1644 1813.2
38.5373 1782 1811.1
38.5427 1760 1808.9
38.5481 1703 1806.7
38.5536 1839 1804.4
38.5590 1733 1802.0
38.5644 1751 1799.7
38.5699 1711 1797.3
38.5753 1713 1795.0
38.5807 1694 1792.6
38.5862 1731 1790.3
38.5916 1742 1788.0
38.5970 1712 1785.9
38.6025 1719 1783.7
38.6079 1698 1781.8
38.6133 1713 1779.8
38.6188 1667 1778.2
38.6242 1657 1776.7
38.6296 1693 1775.4
38.6351 1737 1774.3
38.6405 1769 1773.4
38.6459 1763 1772.8
38.6514 1683 1772.4
38.6568 1679 1772.3
38.6622 1762 1772.5
38.6677 1701 1772.9
38.6731 1697 1773.7
38.6785 1631 1774.8
38.6840 1670 1776.1
38.6894 1686 1777.6
38.6948 1835 1779.4
38.7003 1660 1781.4
38.7057 1691 1783.7
38.7111 1751 1786.2
38.7166 1753 1789.0
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38.7274 1765 1795.2
38.7329 1729 1798.5
38.7383 1727 1802.0
38.7437 1789 1805.6
38.7492 1777 1809.4
38.7546 1666 1813.1
38.7600 1755 1816.9
38.7655 1738 1820.8
38.7709 1754 1824.6
38.7763 1787 1828.4
38.7818 1765 1832.1
38.7872 1823 1835.7
38.7926 1722 1839.2
38.7981 1784 1842.6
38.8035 1822 1845.9
38.8089 1778 1848.9
38.8144 1821 1851.9
38.8198 1820 1854.6
38.8252 1824 1857.2
38.8307 1745 1859.6
38.8361 1747 1862.0
38.8415 1822 1864.1
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38.8524 1743 1868.0
38.8578 1809 1869.8
38.8633 1875 1871.4
38.8687 1801 1873.1
38.8741 1732 1874.6
38.8796 1828 1876.2
38.8850 1731 1877.7
38.8904 1772 1879.3
38.8959 1734 1880.9
38.9013 1753 1882.6
38.9067 1802 1884.4
38.9122 1793 1886.3
38.9176 1854 1888.3
38.9230 1856 1890.5
38.9285 1717 1892.8
38.9339 1848 1895.3
38.9393 1828 1898.1
38.9448 1757 1901.1
38.9502 1764 1904.3
38.9556 1872 1907.8
38.9611 1928 1911.6
38.9665 1855 1915.8
38.9719 1894 1920.2
38.9774 1889 1925.0
38.9828 1961 1930.2
38.9882 1882 1935.7
38.9937 1938 1941.6
38.9991 1971 1947.8
39.0045 2048 1954.5
39.0100 1954 1961.4
39.0154 1985 1968.7
39.0208 1987 1976.4
39.0263 2028 1984.3
39.0317 2017 1992.5
39.0371 2067 2001.0
39.0426 1966 2009.8
39.0480 2133 2018.7
39.0534 2105 2027.8
39.0589 2100 2037.0
39.0643 2114 2046.3
39.0697 2143 2055.6
39.0752 2109 2064.9
39.0806 2120 2074.2
39.0860 2278 2083.3
39.0915 2106 2092.3
39.0969 2215 2101.0
39.1023 2167 2109.5
39.1078 2246 2117.7
39.1132 2248 2125.6
39.1186 2180 2133.0
39.1241 2318 2140.1
39.1295 2255 2146.8
39.1349 2294 2153.1
39.1404 2355 2158.9
39.1458 2371 2164.2
39.1512 2359 2169.1
39.1567 2270 2173.6
39.1621 2273 2177.7
39.1675 2298 2181.3
39.1730 2303 2184.6
39.1784 2284 2187.5
39.1838 2292 2190.1
39.1893 2154 2192.5
39.1947 2212 2194.7
39.2001 2225 2196.6
39.2056 2286 2198.3
39.2110 2251 2199.9
39.2164 2250 2201.5
39.2219 2285 2202.9
39.2273 2225 2204.4
39.2327 2194 2205.9
39.2382 2360 2207.4
39.2436 2309 2209.1
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39.2545 2193 2213.1
39.2599 2303 2215.4
39.2653 2222 2218.1
39.2708 2255 2221.1
39.2762 2216 2224.5
39.2816 2220 2228.4
39.2871 2337 2232.7
39.2925 2351 2237.6
39.2979 2133 2243.0
39.3034 2163 2249.0
39.3088 2285 2255.6
39.3142 2208 2263.0
39.3197 2300 2271.0
39.3251 2216 2279.8
39.3305 2333 2289.3
39.3360 2213 2299.6
39.3414 2366 2310.6
39.3468 2335 2322.4
39.3523 2256 2335.0
39.3577 2369 2348.3
39.3631 2237 2362.4
39.3686 2306 2377.2
39.3740 2368 2392.7
39.3794 2277 2408.9
39.3849 2370 2425.8
39.3903 2286 2443.2
39.3957 2391 2461.2
39.4012 2486 2479.8
39.4066 2390 2498.9
39.4120 2480 2518.4
39.4175 2516 2538.3
39.4229 2553 2558.4
39.4283 2595 2578.6
39.4338 2623 2599.0
39.4392 2594 2619.3
39.4446 2628 2639.5
39.4501 2707 2659.4
39.4555 2682 2679.0
39.4609 2684 2698.1
39.4664 2740 2716.7
39.4718 2888 2734.7
39.4772 2803 2752.0
39.4827 2852 2768.5
39.4881 2810 2784.1
39.4935 2874 2798.7
39.4990 2836 2812.3
39.5044 2994 2824.9
39.5098 2888 2836.2
39.5153 2948 2846.4
39.5207 2878 2855.5
39.5261 2939 2863.4
39.5316 2975 2870.1
39.5370 3001 2875.6
39.5424 3046 2879.9
39.5479 3033 2883.0
39.5533 3019 2885.0
39.5587 3044 2885.8
39.5642 3104 2885.4
39.5696 3041 2883.8
39.5750 3060 2881.1
39.5805 2984 2877.4
39.5859 3052 2872.6
39.5913 2986 2866.7
39.5968 3132 2859.7
39.6022 3132 2851.8
39.6076 3015 2842.7
39.6131 2960 2832.7
39.6185 3000 2821.6
39.6239 2950 2809.6
39.6294 2862 2796.7
39.6348 2994 2782.8
39.6402 3040 2768.1
39.6457 2952 2752.5
39.6511 2941 2736.2
39.6565 3007 2719.1
39.6620 2999 2701.4
39.6674 2803 2683.1
39.6728 2925 2664.2
39.6783 2819 2644.9
39.6837 2816 2625.1
39.6891 2838 2605.0
39.6946 2784 2584.6
39.7000 2896 2563.9
39.7054 2669 2543.0
39.7109 2719 2522.0
39.7163 2703 2500.8
39.7217 2688 2479.6
39.7272 2589 2458.4
39.7326 2677 2437.2
39.7380 2655 2416.1
39.7435 2499 2395.0
39.7489 2517 2374.0
39.7543 2470 2353.0
39.7598 2477 2332.3
39.7652 2508 2311.7
39.7706 2477 2291.3
39.7761 2503 2271.1
39.7815 2497 2251.1
39.7869 2400 2231.5
39.7924 2398 2212.1
39.7978 2323 2193.0
39.8032 2363 2174.3
39.8087 2319 2155.8
39.8141 2359 2137.8
39.8195 2178 2120.0
39.8250 2187 2102.7
39.8304 2243 2085.8
39.8358 2124 2069.3
39.8413 2163 2053.1
39.8467 2254 2037.2
39.8521 2142 2021.7
39.8576 2157 2006.5
39.8630 2103 1991.8
39.8684 2137 1977.4
39.8739 2184 1963.4
39.8793 2043 1949.7
39.8847 2046 1936.4
39.8902 2002 1923.5
39.8956 1937 1910.9
39.9010 2033 1898.7
39.9065 1991 1886.8
39.9119 1952 1875.2
39.9173 2042 1863.9
39.9228 1971 1852.9
39.9282 1796 1842.3
39.9336 1931 1831.9
39.9391 1964 1821.8
39.9445 1864 1812.0
39.9499 1871 1802.6
39.9554 1884 1793.4
39.9608 1816 1784.5
39.9662 1809 1775.9
39.9717 1873 1767.5
39.9771 1814 1759.4
39.9825 1831 1751.6
39.9879 1786 1744.0
39.9934 1804 1736.6
39.9988 1745 1729.5
40.0042 1814 1722.6
40.0097 1827 1715.9
40.0151 1803 1709.5
40.0205 1682 1703.3
40.0260 1784 1697.3
40.0314 1729 1691.5
40.0368 1796 1685.9
40.0423 1711 1680.5
40.0477 1698 1675.3
40.0531 1696 1670.4
40.0586 1691 1665.6
40.0640 1788 1661.0
40.0694 1725 1656.5
40.0749 1727 1652.3
40.0803 1713 1648.2
40.0857 1689 1644.2
40.0912 1643 1640.5
40.0966 1710 1636.8
40.1020 1744 1633.4
40.1075 1722 1630.2
40.1129 1679 1627.1
40.1183 1621 1624.1
40.1238 1749 1621.3
40.1292 1674 1618.7
40.1346 1602 1616.2
40.1401 1643 1613.9
40.1455 1616 1611.7
40.1509 1663 1609.6
40.1564 1677 1607.7
40.1618 1678 1605.9
40.1672 1669 1604.2
40.1727 1569 1602.7
40.1781 1697 1601.3
40.1835 1674 1600.1
40.1890 1627 1599.0
40.1944 1601 1598.0
40.1998 1627 1597.2
40.2053 1635 1596.5
40.2107 1641 1595.9
40.2161 1583 1595.5
40.2216 1679 1595.2
40.2270 1595 1595.0
40.2324 1653 1595.1
40.2379 1653 1595.3
40.2433 1569 1595.7
40.2487 1611 1596.2
40.2542 1639 1596.9
40.2596 1545 1597.8
40.2650 1640 1599.0
40.2705 1546 1600.3
40.2759 1617 1601.8
40.2813 1636 1603.6
40.2868 1621 1605.5
40.2922 1590 1607.6
40.2976 1679 1610.0
40.3031 1609 1612.6
40.3085 1654 1615.4
40.3139 1656 1618.4
40.3194 1613 1621.6
40.3248 1621 1625.1
40.3302 1714 1628.8
40.3357 1661 1632.8
40.3411 1644 1637.1
40.3465 1634 1641.6
40.3520 1645 1646.3
40.3574 1622 1651.3
40.3628 1672 1656.6
40.3683 1648 1662.1
40.3737 1758 1668.1
40.3791 1632 1674.3
40.3846 1700 1680.8
40.3900 1746 1687.6
40.3954 1714 1694.7
40.4009 1721 1702.1
40.4063 1800 1709.8
40.4117 1732 1717.8
40.4172 1840 1726.0
40.4226 1793 1734.5
40.4280 1689 1743.3
40.4335 1734 1752.4
40.4389 1716 1761.7
40.4443 1751 1771.3
40.4498 1812 1781.2
40.4552 1846 1791.3
40.4606 1837 1801.7
40.4661 1797 1812.3
40.4715 1794 1823.2
40.4769 1851 1834.4
40.4824 1860 1845.7
40.4878 1861 1857.4
40.4932 1867 1869.2
40.4987 1944 1881.2
40.5041 2000 1893.3
40.5095 1903 1905.6
40.5150 1878 1918.3
40.5204 1916 1931.2
40.5258 1886 1944.1
40.5313 1990 1957.2
40.5367 1907 1970.3
40.5421 1966 1983.5
40.5476 1868 1996.7
40.5530 2032 2009.8
40.5584 2061 2022.8
40.5639 1957 2035.7
40.5693 2037 2048.4
40.5747 2112 2060.8
40.5802 2080 2072.9
40.5856 2036 2084.6
40.5910 2111 2095.9
40.5965 2072 2106.7
40.6019 2157 2116.9
40.6073 2040 2126.5
40.6128 2031 2135.4
40.6182 2134 2143.5
40.6236 2223 2150.9
40.6291 2187 2157.4
40.6345 2174 2163.0
40.6399 2148 2167.7
40.6454 2091 2171.5
40.6508 2073 2174.3
40.6562 2123 2176.2
40.6617 2187 2177.2
40.6671 2182 2177.3
40.6725 2183 2176.4
40.6780 2178 2174.6
40.6834 2218 2171.9
40.6888 2205 2168.3
40.6943 2111 2164.0
40.6997 2235 2158.9
40.7051 2135 2153.0
40.7106 2135 2146.4
40.7160 2165 2139.2
40.7214 2114 2131.4
40.7269 2125 2123.0
40.7323 2165 2114.0
40.7377 2080 2104.4
40.7432 2160 2094.4
40.7486 2093 2084.0
40.7540 2054 2073.3
40.7595 2136 2062.2
40.7649 2164 2050.7
40.7703 2118 2039.1
40.7758 2033 2027.2
40.7812 2136 2015.2
40.7866 2037 2003.0
40.7921 2041 1990.9
40.7975 1982 1978.7
40.8029 1972 1966.4
40.8084 2068 1954.3
40.8138 2003 1942.2
40.8192 1945 1930.2
40.8247 1965 1918.4
40.8301 1985 1906.9
40.8355 1977 1895.6
40.8410 1951 1884.5
40.8464 1909 1873.7
40.8518 1927 1863.2
40.8573 1966 1853.0
40.8627 1841 1843.2
40.8681 1895 1833.7
40.8736 1945 1824.5
40.8790 1822 1815.6
40.8844 1801 1807.1
40.8899 1885 1799.0
40.8953 1904 1791.1
40.9007 1822 1783.5
40.9062 1807 1776.3
40.9116 1887 1769.3
40.9170 1795 1762.6
40.9225 1789 1756.1
40.9279 1816 1749.9
40.9333 1782 1743.9
40.9388 1784 1738.1
40.9442 1804 1732.5
40.9496 1710 1727.0
40.9551 1793 1721.7
40.9605 1721 1716.6
40.9659 1749 1711.5
40.9714 1729 1706.6
40.9768 1728 1701.8
40.9822 1740 1697.1
40.9877 1682 1692.4
40.9931 1738 1687.9
40.9985 1632 1683.5
41.0040 1727 1679.1
41.0094 1705 1674.8
41.0148 1650 1670.6
41.0203 1697 1666.5
41.0257 1743 1662.4
41.0311 1652 1658.5
41.0366 1703 1654.6
41.0420 1666 1650.8
41.0474 1681 1647.1
41.0529 1574 1643.5
41.0583 1687 1639.9
41.0637 1644 1636.5
41.0692 1646 1633.1
41.0746 1733 1629.9
41.0800 1699 1626.7
41.0855 1687 1623.7
41.0909 1690 1620.7
41.0963 1647 1617.9
41.1018 1620 1615.3
41.1072 1593 1612.8
41.1126 1577 1610.4
41.1181 1617 1608.2
41.1235 1651 1606.0
41.1289 1638 1604.0
41.1344 1622 1602.1
41.1398 1620 1600.4
41.1452 1618 1598.8
41.1507 1566 1597.4
41.1561 1624 1596.3
41.1615 1597 1595.2
41.1670 1621 1594.4
41.1724 1573 1593.8
41.1778 1600 1593.3
41.1833 1591 1593.0
41.1887 1606 1592.9
41.1941 1617 1593.0
41.1996 1651 1593.3
41.2050 1652 1593.7
41.2104 1581 1594.3
41.2159 1576 1595.2
41.2213 1520 1596.2
41.2267 1572 1597.4
41.2322 1566 1598.8
41.2376 1549 1600.3
41.2430 1574 1602.0
41.2485 1595 1603.8
41.2539 1539 1605.7
41.2593 1532 1607.8
41.2648 1591 1609.9
41.2702 1614 1612.2
41.2756 1637 1614.5
41.2811 1525 1616.9
41.2865 1624 1619.4
41.2919 1561 1621.9
41.2974 1578 1624.5
41.3028 1601 1627.0
41.3082 1608 1629.6
41.3137 1616 1632.2
41.3191 1498 1634.7
41.3245 1597 1637.2
41.3300 1532 1639.7
41.3354 1629 1642.1
41.3408 1605 1644.4
41.3463 1540 1646.7
41.3517 1566 1648.9
41.3571 1569 1651.1
41.3626 1590 1653.2
41.3680 1683 1655.2
41.3734 1546 1657.1
41.3789 1583 1659.0
41.3843 1619 1660.8
41.3897 1625 1662.6
41.3952 1609 1664.3
41.4006 1625 1665.9
41.4060 1550 1667.6
41.4115 1637 1669.2
41.4169 1621 1670.9
41.4223 1607 1672.5
41.4278 1651 1674.2
41.4332 1608 1675.9
41.4386 1540 1677.6
41.4441 1605 1679.4
41.4495 1633 1681.3
41.4549 1699 1683.2
41.4604 1650 1685.3
41.4658 1638 1687.4
41.4712 1616 1689.8
41.4767 1670 1692.2
41.4821 1635 1694.9
41.4875 1623 1697.7
41.4930 1643 1700.7
41.4984 1612 1703.9
41.5038 1685 1707.3
41.5093 1749 1711.0
41.5147 1628 1714.9
41.5201 1719 1719.1
41.5256 1680 1723.6
41.5310 1658 1728.4
41.5364 1643 1733.4
41.5419 1705 1738.8
41.5473 1660 1744.6
41.5527 1726 1750.6
41.5582 1712 1757.1
41.5636 1752 1763.8
41.5690 1693 1771.0
41.5744 1767 1778.4
41.5799 1702 1786.2
41.5853 1809 1794.5
41.5907 1827 1803.0
41.5962 1804 1812.1
41.6016 1797 1821.5
41.6070 1804 1831.4
41.6125 1837 1841.7
41.6179 1849 1852.3
41.6233 1730 1863.4
41.6288 1846 1874.8
41.6342 1906 1886.7
41.6396 1811 1898.8
41.6451 1918 1911.4
41.6505 2028 1924.3
41.6559 1878 1937.7
41.6614 1896 1951.3
41.6668 1967 1965.4
41.6722 1929 1979.8
41.6777 2025 1994.6
41.6831 1888 2009.8
41.6885 2017 2025.2
41.6940 2033 2040.9
41.6994 1979 2057.0
41.7048 2047 2073.3
41.7103 2118 2089.9
41.7157 2058 2106.8
41.7211 2070 2123.9
41.7266 2068 2141.1
41.7320 2143 2158.6
41.7374 2193 2176.2
41.7429 2136 2193.8
41.7483 2154 2211.6
41.7537 2153 2229.3
41.7592 2195 2246.9
41.7646 2265 2264.4
41.7700 2244 2281.7
41.7755 2198 2298.8
41.7809 2228 2315.6
41.7863 2307 2332.0
41.7918 2365 2347.9
41.7972 2243 2363.4
41.8026 2357 2378.3
41.8081 2303 2392.6
41.8135 2429 2406.2
41.8189 2418 2419.0
41.8244 2362 2431.1
41.8298 2370 2442.3
41.8352 2354 2452.7
41.8407 2277 2462.2
41.8461 2383 2470.7
41.8515 2389 2478.4
41.8570 2416 2485.1
41.8624 2491 2490.9
41.8678 2458 2495.7
41.8733 2464 2499.5
41.8787 2494 2502.4
41.8841 2466 2504.2
41.8896 2457 2505.2
41.8950 2543 2505.2
41.9004 2492 2504.3
41.9059 2507 2502.4
41.9113 2563 2499.7
41.9167 2530 2496.1
41.9222 2488 2491.5
41.9276 2547 2486.1
41.9330 2518 2479.9
41.9385 2513 2472.7
41.9439 2488 2464.7
41.9493 2535 2455.8
41.9548 2408 2446.2
41.9602 2452 2435.7
41.9656 2523 2424.4
41.9711 2404 2412.4
41.9765 2476 2399.7
41.9819 2514 2386.3
41.9874 2368 2372.2
41.9928 2298 2357.6
41.9982 2404 2342.4
42.0037 2322 2326.6
42.0091 2303 2310.4
42.0145 2323 2293.8
42.0200 2355 2276.8
42.0254 2265 2259.4
42.0308 2183 2241.8
42.0363 2225 2224.0
42.0417 2328 2205.9
42.0471 2287 2187.7
42.0526 2192 2169.4
42.0580 2230 2151.0
42.0634 2151 2132.6
42.0689 2286 2114.2
42.0743 2094 2095.8
42.0797 2090 2077.5
42.0852 2111 2059.2
42.0906 2049 2041.1
42.0960 2083 2023.0
42.1015 2048 2005.1
42.1069 2012 1987.4
42.1123 1974 1969.9
42.1178 2045 1952.6
42.1232 2013 1935.5
42.1286 1929 1918.6
42.1341 1973 1902.1
42.1395 1883 1885.8
42.1449 1885 1869.8
42.1504 1865 1854.0
42.1558 1867 1838.6
42.1612 1936 1823.6
42.1667 1830 1808.9
42.1721 1860 1794.5
42.1775 1882 1780.6
42.1830 1779 1766.9
42.1884 1717 1753.7
42.1938 1748 1740.8
42.1993 1741 1728.3
42.2047 1759 1716.1
42.2101 1710 1704.3
42.2156 1760 1692.9
42.2210 1674 1681.8
42.2264 1615 1671.1
42.2319 1606 1660.8
42.2373 1707 1650.8
42.2427 1653 1641.1
42.2482 1665 1631.8
42.2536 1653 1622.8
42.2590 1614 1614.1
42.2645 1604 1605.7
42.2699 1594 1597.6
42.2753 1629 1589.8
42.2808 1590 1582.3
42.2862 1511 1575.1
42.2916 1604 1568.2
42.2971 1614 1561.6
42.3025 1578 1555.1
42.3079 1503 1549.0
42.3134 1488 1543.0
42.3188 1556 1537.3
42.3242 1487 1531.9
42.3297 1580 1526.6
42.3351 1519 1521.5
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53.5004 1492 1399.5
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53.5112 1436 1403.3
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53.5221 1425 1408.1
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53.5330 1458 1413.9
53.5384 1504 1417.1
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53.5493 1489 1424.4
53.5547 1453 1428.4
53.5601 1517 1432.7
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53.5819 1554 1452.2
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53.6253 1639 1502.8
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53.6742 1580 1575.0
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53.6851 1600 1592.5
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53.7068 1629 1628.0
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53.7775 1872 1736.3
53.7829 1841 1743.6
53.7883 1836 1750.6
53.7938 1848 1757.5
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53.8101 1893 1777.0
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53.8264 1851 1794.7
53.8318 1820 1800.3
53.8372 1919 1805.7
53.8427 1825 1811.0
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53.8535 1833 1820.9
53.8590 1891 1825.6
53.8644 1908 1830.1
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53.8807 1912 1842.4
53.8861 1856 1846.0
53.8916 1900 1849.5
53.8970 1989 1852.7
53.9024 2031 1855.6
53.9079 1953 1858.2
53.9133 1982 1860.5
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53.9242 1917 1864.1
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53.9513 1968 1866.4
53.9568 1982 1865.6
53.9622 1933 1864.3
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53.9731 2035 1860.4
53.9785 2000 1857.8
53.9839 2012 1854.7
53.9894 2000 1851.2
53.9948 2039 1847.2
54.0002 1975 1842.9
54.0057 2000 1838.1
54.0111 2045 1832.9
54.0165 1982 1827.3
54.0220 2027 1821.4
54.0274 2045 1815.1
54.0328 2019 1808.5
54.0383 1972 1801.6
54.0437 1963 1794.4
54.0491 1901 1787.0
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54.0600 1974 1771.4
54.0654 1960 1763.3
54.0709 1960 1755.0
54.0763 1919 1746.5
54.0817 2006 1737.8
54.0872 1905 1729.0
54.0926 1899 1720.1
54.0980 1871 1711.0
54.1035 1887 1701.9
54.1089 1869 1692.6
54.1143 1853 1683.3
54.1198 1801 1673.8
54.1252 1801 1664.4
54.1306 1934 1654.8
54.1361 1752 1645.2
54.1415 1753 1635.6
54.1469 1771 1625.9
54.1524 1813 1616.2
54.1578 1830 1606.5
54.1632 1804 1596.8
54.1687 1796 1587.1
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54.1795 1691 1568.0
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54.3045 1421 1385.8
54.3099 1460 1380.1
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54.3262 1451 1364.2
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54.3371 1413 1354.7
54.3425 1391 1350.1
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55.2227 1146 1186.2
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55.2499 1162 1180.1
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56.6679 1073 1080.6
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56.9559 1103 1080.6
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57.1026 1090 1104.6
57.1080 1105 1105.8
57.1135 1111 1107.1
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57.1298 1101 1111.1
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57.2113 1138 1136.1
57.2167 1177 1138.0
57.2221 1128 1139.9
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64.6874 843 798.3
64.6928 801 798.3
64.6982 802 798.3
64.7037 843 798.2
64.7091 812 798.2
64.7145 757 798.2
64.7200 794 798.1
64.7254 782 798.1
64.7308 814 798.0
64.7363 800 798.0
64.7417 824 797.9
64.7471 789 797.8
64.7526 797 797.7
64.7580 756 797.6
64.7634 736 797.5
64.7689 832 797.4
64.7743 828 797.3
64.7797 778 797.2
64.7852 754 797.1
64.7906 774 796.9
64.7960 785 796.8
64.8015 791 796.6
64.8069 771 796.5
64.8123 790 796.3
64.8178 800 796.2
64.8232 731 796.0
64.8286 746 795.8
64.8341 765 795.6
64.8395 834 795.5
64.8449 776 795.3
64.8504 822 795.1
64.8558 776 794.9
64.8612 819 794.7
64.8667 818 794.5
64.8721 768 794.3
64.8775 806 794.1
64.8830 843 793.9
64.8884 794 793.7
64.8938 808 793.5
64.8993 773 793.3
64.9047 830 793.1
64.9101 837 792.9
64.9156 785 792.7
64.9210 842 792.5
64.9264 810 792.3
64.9319 780 792.1
64.9373 837 791.9
64.9427 834 791.7
64.9482 795 791.5
64.9536 841 791.3
64.9590 788 791.1
64.9645 836 790.8
64.9699 814 790.6
64.9753 855 790.4
64.9808 829 790.2
64.9862 822 789.9
64.9916 824 789.7
64.9971 796 789.4
65.0025 790 789.2
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_new_knoaven_2_P21n
_database_code_depnum_ccdc_archive 'CCDC 1869002'
_audit_update_record             
;
2018-10-23 deposited with the CCDC.
2018-10-30 downloaded from the CCDC.
;


_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            'Knoevengel prod hemihydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 N2 O5, 0.5(H2 O)'
_chemical_formula_sum            'C12 H11 N2 O5.5'
_chemical_formula_weight         271.2
_chemical_oxdiff_formula         C12H10N2O5
_chemical_oxdiff_usercomment     "Tiny crystal with poor diffraction'"

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.148(4)
_cell_length_b                   14.7902(14)
_cell_length_c                   12.1137(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.972(15)
_cell_angle_gamma                90.00
_cell_volume                     2278.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    126.3(6)
_cell_measurement_reflns_used    770
_cell_measurement_theta_min      5.0320
_cell_measurement_theta_max      74.6430

_exptl_crystal_description       block
_exptl_crystal_colour            yellow-orange
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1138
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.31634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      126.3(6)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         
'micro-focus sealed X-ray tube, Nova (Cu) X-ray Source '
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  
'four-circle diffractometer Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4323
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11607
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_sigmaI/netI    0.1684
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.9878
_diffrn_reflns_theta_max         75.85
_reflns_number_total             4672
_reflns_number_gt                2342
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'ShelX-97(Sheldrick, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0795P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4672
_refine_ls_number_parameters     366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.2288
_refine_ls_wR_factor_gt          0.1808
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.989
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O03 O 0.3445(3) 0.34965(19) -0.7963(3) 0.0344(7) Uani 1 1 d . . .
O07 O 0.3671(3) 0.12839(18) 0.1069(3) 0.0319(7) Uani 1 1 d . . .
O06 O 0.3368(3) 0.3888(2) -0.0965(3) 0.0392(8) Uani 1 1 d . . .
O08 O 0.3389(3) 0.1351(2) -0.2999(3) 0.0354(7) Uani 1 1 d . . .
O04 O 0.4055(3) 0.7835(2) -0.3502(3) 0.0371(7) Uani 1 1 d . . .
H4O H 0.4024 0.8272 -0.3933 0.056 Uiso 1 1 calc R . .
O05 O 0.4211(3) 0.6339(2) -0.2327(3) 0.0387(8) Uani 1 1 d . . .
O02 O 0.3763(3) 0.3501(2) -0.3880(3) 0.0410(8) Uani 1 1 d . . .
O01 O 0.3385(3) 0.09285(19) -0.5997(3) 0.0417(8) Uani 1 1 d . . .
O10 O 0.4191(3) -0.1585(2) 0.2580(3) 0.0371(7) Uani 1 1 d . . .
O09 O 0.4193(3) -0.3067(2) 0.1356(4) 0.0474(9) Uani 1 1 d . . .
H5O H 0.4252 -0.2991 0.2054 0.071 Uiso 1 1 calc R . .
N01 N 0.3469(3) 0.2232(2) -0.6935(4) 0.0296(7) Uani 1 1 d . . .
H01N H 0.3457 0.1925 -0.7544 0.036 Uiso 1 1 calc R . .
N03 N 0.3530(3) 0.2556(2) 0.0021(4) 0.0314(8) Uani 1 1 d . . .
H03N H 0.3548 0.2843 0.0647 0.038 Uiso 1 1 calc R . .
N04 N 0.3417(3) 0.2604(2) -0.1942(4) 0.0297(8) Uani 1 1 d . . .
H04N H 0.3379 0.2916 -0.2558 0.036 Uiso 1 1 calc R . .
N02 N 0.3534(3) 0.2252(2) -0.4989(4) 0.0310(8) Uani 1 1 d . . .
H02N H 0.3514 0.1962 -0.4385 0.037 Uiso 1 1 calc R . .
O2W O 0.3339(4) 0.9395(3) -0.4564(5) 0.0452(11) Uani 0.83 1 d PG . .
H2WB H 0.3421 0.9881 -0.4889 0.068 Uiso 0.83 1 d PG . .
H2WA H 0.2715 0.9374 -0.4631 0.068 Uiso 0.83 1 d PG . .
C15 C 0.3546(3) 0.1139(3) -0.0964(4) 0.0290(8) Uani 1 1 d . . .
C03 C 0.3584(3) 0.3679(3) -0.5940(4) 0.0272(8) Uani 1 1 d . . .
C06 C 0.3754(3) 0.5398(3) -0.5351(4) 0.0284(9) Uani 1 1 d . . .
C16 C 0.3445(3) 0.1674(3) -0.2039(4) 0.0278(8) Uani 1 1 d . . .
C19 C 0.3757(4) -0.1384(3) -0.1007(4) 0.0305(9) Uani 1 1 d . . .
H19C H 0.3669 -0.1361 -0.1814 0.037 Uiso 1 1 calc R . .
C02 C 0.3494(3) 0.3150(3) -0.7018(4) 0.0288(9) Uani 1 1 d . . .
C14 C 0.3590(3) 0.1628(3) 0.0114(4) 0.0285(8) Uani 1 1 d . . .
C08 C 0.4043(4) 0.6249(3) -0.3517(4) 0.0306(9) Uani 1 1 d . . .
C17 C 0.3604(3) 0.0232(3) -0.1122(4) 0.0298(9) Uani 1 1 d . . .
H17C H 0.3532 0.0101 -0.1906 0.036 Uiso 1 1 calc R . .
C04 C 0.3639(4) 0.3181(3) -0.4873(4) 0.0307(9) Uani 1 1 d . . .
C05 C 0.3634(3) 0.4601(3) -0.6060(4) 0.0294(9) Uani 1 1 d . . .
H05C H 0.3569 0.4747 -0.6836 0.035 Uiso 1 1 calc R . .
C18 C 0.3746(3) -0.0582(3) -0.0410(4) 0.0298(9) Uani 1 1 d . . .
C22 C 0.4041(4) -0.1459(3) 0.1403(4) 0.0308(9) Uani 1 1 d . . .
C20 C 0.3896(4) -0.2219(3) -0.0427(5) 0.0365(10) Uani 1 1 d . . .
H20C H 0.3898 -0.2745 -0.0846 0.044 Uiso 1 1 calc R . .
C23 C 0.3881(3) -0.0634(3) 0.0816(4) 0.0308(9) Uani 1 1 d . . .
H23C H 0.3861 -0.0110 0.1229 0.037 Uiso 1 1 calc R . .
C09 C 0.3955(3) 0.7071(3) -0.4141(4) 0.0295(9) Uani 1 1 d . . .
C07 C 0.3938(3) 0.5431(3) -0.4107(4) 0.0298(9) Uani 1 1 d . . .
H07C H 0.3988 0.4896 -0.3682 0.036 Uiso 1 1 calc R . .
C11 C 0.3703(4) 0.6223(3) -0.5941(4) 0.0313(9) Uani 1 1 d . . .
H11C H 0.3603 0.6217 -0.6753 0.038 Uiso 1 1 calc R . .
C21 C 0.4033(4) -0.2264(3) 0.0777(5) 0.0341(9) Uani 1 1 d . . .
C13 C 0.3444(4) 0.3074(3) -0.0955(4) 0.0316(9) Uani 1 1 d . . .
C01 C 0.3459(4) 0.1751(3) -0.5974(4) 0.0310(9) Uani 1 1 d . . .
C10 C 0.3796(4) 0.7047(3) -0.5362(5) 0.0327(9) Uani 1 1 d . . .
H10C H 0.3753 0.7583 -0.5784 0.039 Uiso 1 1 calc R . .
C24 C 0.4315(5) -0.0779(3) 0.3281(5) 0.0419(11) Uani 1 1 d . . .
H24B H 0.3679 -0.0430 0.2923 0.063 Uiso 1 1 calc R . .
H24A H 0.4886 -0.0429 0.3280 0.063 Uiso 1 1 calc R . .
H24C H 0.4462 -0.0936 0.4110 0.063 Uiso 1 1 calc R . .
C12 C 0.4375(6) 0.5526(3) -0.1643(5) 0.0572(17) Uani 1 1 d . . .
H12C H 0.3748 0.5165 -0.1988 0.086 Uiso 1 1 calc R . .
H12A H 0.4540 0.5668 -0.0805 0.086 Uiso 1 1 calc R . .
H12B H 0.4947 0.5195 -0.1673 0.086 Uiso 1 1 calc R . .
O1W O 0.3315(12) 0.5516(6) 0.0030(13) 0.042(5) Uani 0.17 1 d PR . .


_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
O03 C02 1.228(5) . ?
O07 C14 1.221(5) . ?
O06 C13 1.208(5) . ?
O08 C16 1.227(5) . ?
O04 C09 1.342(5) . ?
O04 H4O 0.8200 . ?
O05 C08 1.360(6) . ?
O05 C12 1.421(5) . ?
O02 C04 1.232(6) . ?
O01 C01 1.220(5) . ?
O10 C22 1.360(6) . ?
O10 C24 1.429(5) . ?
O09 C21 1.347(6) . ?
O09 H5O 0.8200 . ?
N01 C02 1.364(5) . ?
N01 C01 1.369(6) . ?
N01 H01N 0.8600 . ?
N03 C13 1.369(6) . ?
N03 C14 1.377(5) . ?
N03 H03N 0.8600 . ?
N04 C13 1.368(6) . ?
N04 C16 1.383(5) . ?
N04 H04N 0.8600 . ?
N02 C01 1.369(6) . ?
N02 C04 1.382(5) . ?
N02 H02N 0.8600 . ?
O2W H2WB 0.8505 . ?
O2W H2WA 0.8500 . ?
C15 C17 1.362(6) . ?
C15 C14 1.470(6) . ?
C15 C16 1.476(6) . ?
C03 C05 1.377(5) . ?
C03 C04 1.459(6) . ?
C03 C02 1.479(6) . ?
C06 C11 1.400(6) . ?
C06 C07 1.413(6) . ?
C06 C05 1.425(6) . ?
C19 C20 1.391(6) . ?
C19 C18 1.393(6) . ?
C19 H19C 0.9300 . ?
C08 C07 1.380(6) . ?
C08 C09 1.408(6) . ?
C17 C18 1.443(6) . ?
C17 H17C 0.9300 . ?
C05 H05C 0.9300 . ?
C18 C23 1.414(6) . ?
C22 C23 1.380(6) . ?
C22 C21 1.409(6) . ?
C20 C21 1.386(7) . ?
C20 H20C 0.9300 . ?
C23 H23C 0.9300 . ?
C09 C10 1.396(7) . ?
C07 H07C 0.9300 . ?
C11 C10 1.384(6) . ?
C11 H11C 0.9300 . ?
C10 H10C 0.9300 . ?
C24 H24B 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24C 0.9600 . ?
C12 H12C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 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
C09 O04 H4O 109.5 . . ?
C08 O05 C12 116.3(4) . . ?
C22 O10 C24 115.5(3) . . ?
C21 O09 H5O 109.5 . . ?
C02 N01 C01 126.2(4) . . ?
C02 N01 H01N 116.9 . . ?
C01 N01 H01N 116.9 . . ?
C13 N03 C14 127.5(4) . . ?
C13 N03 H03N 116.3 . . ?
C14 N03 H03N 116.3 . . ?
C13 N04 C16 126.1(4) . . ?
C13 N04 H04N 117.0 . . ?
C16 N04 H04N 117.0 . . ?
C01 N02 C04 126.2(4) . . ?
C01 N02 H02N 116.9 . . ?
C04 N02 H02N 116.9 . . ?
H2WB O2W H2WA 109.5 . . ?
C17 C15 C14 128.9(4) . . ?
C17 C15 C16 113.1(4) . . ?
C14 C15 C16 118.0(4) . . ?
C05 C03 C04 127.4(4) . . ?
C05 C03 C02 114.8(4) . . ?
C04 C03 C02 117.8(3) . . ?
C11 C06 C07 117.3(4) . . ?
C11 C06 C05 116.6(4) . . ?
C07 C06 C05 126.1(4) . . ?
O08 C16 N04 118.4(4) . . ?
O08 C16 C15 124.7(4) . . ?
N04 C16 C15 117.0(4) . . ?
C20 C19 C18 121.6(4) . . ?
C20 C19 H19C 119.2 . . ?
C18 C19 H19C 119.2 . . ?
O03 C02 N01 119.4(4) . . ?
O03 C02 C03 123.4(4) . . ?
N01 C02 C03 117.1(4) . . ?
O07 C14 N03 118.0(4) . . ?
O07 C14 C15 125.9(4) . . ?
N03 C14 C15 116.1(4) . . ?
O05 C08 C07 124.3(4) . . ?
O05 C08 C09 114.7(4) . . ?
C07 C08 C09 120.9(4) . . ?
C15 C17 C18 137.6(4) . . ?
C15 C17 H17C 111.2 . . ?
C18 C17 H17C 111.2 . . ?
O02 C04 N02 116.3(4) . . ?
O02 C04 C03 126.9(4) . . ?
N02 C04 C03 116.7(4) . . ?
C03 C05 C06 139.0(4) . . ?
C03 C05 H05C 110.5 . . ?
C06 C05 H05C 110.5 . . ?
C19 C18 C23 118.2(4) . . ?
C19 C18 C17 115.5(4) . . ?
C23 C18 C17 126.3(4) . . ?
O10 C22 C23 125.2(4) . . ?
O10 C22 C21 114.2(4) . . ?
C23 C22 C21 120.6(4) . . ?
C21 C20 C19 119.9(4) . . ?
C21 C20 H20C 120.0 . . ?
C19 C20 H20C 120.0 . . ?
C22 C23 C18 120.3(4) . . ?
C22 C23 H23C 119.8 . . ?
C18 C23 H23C 119.8 . . ?
O04 C09 C10 124.1(4) . . ?
O04 C09 C08 117.0(4) . . ?
C10 C09 C08 118.9(4) . . ?
C08 C07 C06 120.7(4) . . ?
C08 C07 H07C 119.7 . . ?
C06 C07 H07C 119.7 . . ?
C10 C11 C06 122.4(4) . . ?
C10 C11 H11C 118.8 . . ?
C06 C11 H11C 118.8 . . ?
O09 C21 C20 120.4(4) . . ?
O09 C21 C22 120.3(4) . . ?
C20 C21 C22 119.3(4) . . ?
O06 C13 N04 121.9(4) . . ?
O06 C13 N03 122.7(4) . . ?
N04 C13 N03 115.3(4) . . ?
O01 C01 N02 122.2(4) . . ?
O01 C01 N01 122.1(4) . . ?
N02 C01 N01 115.7(4) . . ?
C11 C10 C09 119.7(4) . . ?
C11 C10 H10C 120.2 . . ?
C09 C10 H10C 120.2 . . ?
O10 C24 H24B 109.5 . . ?
O10 C24 H24A 109.5 . . ?
H24B C24 H24A 109.5 . . ?
O10 C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
O05 C12 H12C 109.5 . . ?
O05 C12 H12A 109.5 . . ?
H12C C12 H12A 109.5 . . ?
O05 C12 H12B 109.5 . . ?
H12C C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        75.85
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.078
