#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:40:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179150 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/11/4311133.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4311133
loop_
_publ_author_name
'Weiqing Zhong'
'John A. Parkinson'
'Simon Parsons'
'Iain D. H. Oswald'
'Robert A. Coxall'
'Peter J. Sadler'
_publ_section_title
;
 Structure and Dynamics of Dinuclear Zirconium(IV) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3561
_journal_page_last               3572
_journal_paper_doi               10.1021/ic049932k
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         Cs2[H5O2][Zr(C11H13N2O9)2Cl].4H2O
_chemical_formula_sum            'C22 H39 Cl Cs2 N4 O24 Zr2'
_chemical_formula_weight         1227.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'geom/difmap (on H2O)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.7080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2765(8)
_cell_length_b                   13.1465(7)
_cell_length_c                   20.1326(11)
_cell_measurement_reflns_used    7710
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.5
_cell_volume                     3686.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20673
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    2.682
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.279
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    'Riding/ restrained refall'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         7510
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0265P)²+7.5307P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                6766
_reflns_number_total             7510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049932ksi20040116_065918.cif
_cod_data_source_block           cszrdp
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multiscan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4311133
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'
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
Cs1 Cs 0.41577(2) 0.21068(2) 0.113380(14) 0.01785(8) Uani 1 1 d . . .
Cs2 Cs 0.68731(2) 0.11412(2) 0.034026(15) 0.02388(8) Uani 1 1 d . . .
Zr1 Zr 1.02075(3) -0.06063(3) 0.160483(19) 0.00783(9) Uani 1 1 d . . .
Zr2 Zr 0.89493(3) 0.04292(3) 0.280441(19) 0.00729(9) Uani 1 1 d . . .
N1 N 1.1917(2) -0.0458(2) 0.21489(17) 0.0102(7) Uani 1 1 d . . .
C1 C 1.1923(3) -0.1760(3) 0.1291(2) 0.0160(9) Uani 1 1 d . . .
C2 C 1.2384(3) -0.1415(3) 0.2009(2) 0.0127(9) Uani 1 1 d . . .
H2A H 1.2301 -0.1943 0.2342 0.015 Uiso 1 1 calc R . .
H2B H 1.3080 -0.1302 0.2051 0.015 Uiso 1 1 calc R . .
N2 N 1.0212(2) 0.1090(2) 0.37126(17) 0.0095(7) Uani 1 1 d . . .
C3 C 1.1993(3) -0.0275(3) 0.2886(2) 0.0115(8) Uani 1 1 d . . .
H3A H 1.2638 -0.0005 0.3095 0.014 Uiso 1 1 calc R . .
H3B H 1.1902 -0.0922 0.3116 0.014 Uiso 1 1 calc R . .
N3 N 0.9185(2) -0.1984(3) 0.10369(17) 0.0103(7) Uani 1 1 d . . .
O4 O 1.03418(19) 0.0124(2) 0.25742(14) 0.0095(6) Uani 1 1 d . . .
N4 N 0.7518(2) -0.0632(3) 0.27390(17) 0.0095(7) Uani 1 1 d . . .
C4 C 1.1229(3) 0.0483(3) 0.2970(2) 0.0107(8) Uani 1 1 d . . .
H4A H 1.1379 0.1169 0.2806 0.013 Uiso 1 1 calc R . .
C5 C 1.1119(3) 0.0551(3) 0.3703(2) 0.0090(8) Uani 1 1 d . . .
H5A H 1.1105 -0.0141 0.3896 0.011 Uiso 1 1 calc R . .
H5B H 1.1669 0.0925 0.3982 0.011 Uiso 1 1 calc R . .
C6 C 0.9921(3) 0.0907(3) 0.4365(2) 0.0121(9) Uani 1 1 d . . .
H6A H 1.0243 0.1405 0.4710 0.015 Uiso 1 1 calc R . .
H6B H 1.0121 0.0216 0.4534 0.015 Uiso 1 1 calc R . .
C7 C 0.8838(3) 0.1011(3) 0.4265(2) 0.0136(9) Uani 1 1 d . . .
C8 C 1.2342(3) 0.0397(3) 0.1833(2) 0.0123(9) Uani 1 1 d . . .
H8A H 1.2631 0.0130 0.1464 0.015 Uiso 1 1 calc R . .
H8B H 1.2861 0.0714 0.2179 0.015 Uiso 1 1 calc R . .
C9 C 1.1605(3) 0.1195(3) 0.1545(2) 0.0121(9) Uani 1 1 d . . .
C10 C 1.0320(3) 0.2204(3) 0.3623(2) 0.0114(8) Uani 1 1 d . . .
H10A H 1.1007 0.2389 0.3769 0.014 Uiso 1 1 calc R . .
H10B H 0.9964 0.2572 0.3918 0.014 Uiso 1 1 calc R . .
O11 O 1.1082(2) -0.1399(2) 0.10373(14) 0.0130(6) Uani 1 1 d . . .
C11 C 0.9953(3) 0.2537(3) 0.2893(2) 0.0123(9) Uani 1 1 d . . .
O12 O 1.2342(2) -0.2377(3) 0.09985(17) 0.0248(8) Uani 1 1 d . . .
C12 C 1.0319(3) -0.2887(3) 0.1940(2) 0.0134(9) Uani 1 1 d . . .
C13 C 0.9691(3) -0.2956(3) 0.1231(2) 0.0116(8) Uani 1 1 d . . .
H13A H 1.0091 -0.3122 0.0902 0.014 Uiso 1 1 calc R . .
H13B H 0.9215 -0.3509 0.1216 0.014 Uiso 1 1 calc R . .
C14 C 0.8232(3) -0.1953(3) 0.1239(2) 0.0112(8) Uani 1 1 d . . .
H14A H 0.7967 -0.2650 0.1230 0.013 Uiso 1 1 calc R . .
H14B H 0.7775 -0.1534 0.0909 0.013 Uiso 1 1 calc R . .
O15 O 0.88790(19) -0.0585(2) 0.19622(14) 0.0095(6) Uani 1 1 d . . .
C15 C 0.8345(3) -0.1510(3) 0.1945(2) 0.0104(8) Uani 1 1 d . . .
H15A H 0.8701 -0.1998 0.2292 0.012 Uiso 1 1 calc R . .
C16 C 0.7388(3) -0.1251(3) 0.2104(2) 0.0105(8) Uani 1 1 d . . .
H16A H 0.6995 -0.0865 0.1720 0.013 Uiso 1 1 calc R . .
H16B H 0.7041 -0.1886 0.2160 0.013 Uiso 1 1 calc R . .
C17 C 0.7649(3) -0.1276(3) 0.3355(2) 0.0133(9) Uani 1 1 d . . .
H17A H 0.7382 -0.1960 0.3226 0.016 Uiso 1 1 calc R . .
H17B H 0.7287 -0.0976 0.3674 0.016 Uiso 1 1 calc R . .
C18 C 0.8702(3) -0.1375(3) 0.3713(2) 0.0118(9) Uani 1 1 d . . .
C19 C 0.9010(3) -0.1773(3) 0.0298(2) 0.0129(9) Uani 1 1 d . . .
H19A H 0.8457 -0.2176 0.0049 0.015 Uiso 1 1 calc R . .
H19B H 0.9583 -0.1951 0.0120 0.015 Uiso 1 1 calc R . .
C20 C 0.8797(3) -0.0633(3) 0.0213(2) 0.0122(9) Uani 1 1 d . . .
C21 C 0.6688(3) 0.0071(3) 0.2666(2) 0.0136(9) Uani 1 1 d . . .
H21A H 0.6634 0.0320 0.3120 0.016 Uiso 1 1 calc R . .
H21B H 0.6088 -0.0295 0.2460 0.016 Uiso 1 1 calc R . .
C22 C 0.6821(3) 0.0963(3) 0.2220(2) 0.0147(9) Uani 1 1 d . . .
O71 O 0.8357(2) 0.0986(2) 0.36378(14) 0.0127(6) Uani 1 1 d . . .
O72 O 0.8479(2) 0.1066(2) 0.47638(15) 0.0193(7) Uani 1 1 d . . .
O91 O 1.0737(2) 0.0910(2) 0.14007(15) 0.0123(6) Uani 1 1 d . . .
O92 O 1.1901(2) 0.2063(2) 0.14468(16) 0.0169(7) Uani 1 1 d . . .
O111 O 0.9372(2) 0.1931(2) 0.25063(14) 0.0123(6) Uani 1 1 d . . .
O112 O 1.0199(2) 0.3373(2) 0.27079(15) 0.0156(6) Uani 1 1 d . . .
O121 O 1.0471(2) -0.1991(2) 0.22028(14) 0.0115(6) Uani 1 1 d . . .
O122 O 1.0686(2) -0.3671(2) 0.22239(16) 0.0209(7) Uani 1 1 d . . .
O181 O 0.93055(19) -0.0862(2) 0.34463(14) 0.0111(6) Uani 1 1 d . . .
O182 O 0.8931(2) -0.1901(2) 0.42196(15) 0.0173(7) Uani 1 1 d . . .
O201 O 0.9331(2) -0.0074(2) 0.06833(14) 0.0141(6) Uani 1 1 d . . .
O202 O 0.8164(2) -0.0311(2) -0.02475(15) 0.0178(7) Uani 1 1 d . . .
O221 O 0.7703(2) 0.1138(2) 0.21870(15) 0.0133(6) Uani 1 1 d . . .
O222 O 0.6139(2) 0.1468(2) 0.19342(18) 0.0248(8) Uani 1 1 d . . .
Cl1 Cl 0.57950(8) -0.11624(9) 0.04218(6) 0.0206(2) Uani 1 1 d . . .
O1W O 0.4234(3) -0.0239(3) 0.11484(19) 0.0240(8) Uani 1 1 d D . .
H1W1 H 0.463(3) -0.041(4) 0.096(3) 0.039(18) Uiso 1 1 d D . .
H2W1 H 0.437(5) -0.060(4) 0.146(2) 0.06(2) Uiso 1 1 d D . .
O2W O 0.8953(3) 0.2159(3) 0.1033(2) 0.0301(9) Uani 1 1 d D . .
H1W2 H 0.930(3) 0.174(3) 0.095(3) 0.030(16) Uiso 1 1 d D . .
H2W2 H 0.897(6) 0.220(6) 0.1420(14) 0.08(3) Uiso 1 1 d D . .
O3W O 1.0143(3) 0.4516(3) 0.15831(19) 0.0259(8) Uani 1 1 d D . .
H1W3 H 1.017(6) 0.413(5) 0.188(3) 0.08(3) Uiso 1 1 d D . .
H2W3 H 1.028(4) 0.505(2) 0.175(3) 0.028(16) Uiso 1 1 d D . .
O4W O 1.0940(3) 0.3528(3) 0.0806(2) 0.0339(9) Uani 1 1 d D . .
H1W4 H 1.130(3) 0.391(3) 0.069(3) 0.018(15) Uiso 1 1 d D . .
H2W4 H 1.053(4) 0.394(4) 0.113(3) 0.024(13) Uiso 1 1 d . . .
H3W4 H 1.137(6) 0.286(7) 0.107(4) 0.10(3) Uiso 1 1 d . . .
O5W O 1.1727(3) 0.4417(3) -0.0018(2) 0.0356(10) Uani 1 1 d D . .
H1W5 H 1.174(5) 0.5008(18) 0.001(3) 0.06(2) Uiso 1 1 d D . .
H2W5 H 1.224(2) 0.433(5) -0.008(3) 0.035(18) Uiso 1 1 d D . .
O6W O 0.8599(4) 0.3627(3) 0.0022(2) 0.0494(13) Uani 1 1 d D . .
H1W6 H 0.836(4) 0.327(4) -0.028(2) 0.043(19) Uiso 1 1 d D . .
H2W6 H 0.873(5) 0.331(5) 0.036(2) 0.06(2) Uiso 1 1 d D . .
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'
N N 0.0061 0.0033 '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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O222 Cs1 O1W 72.14(9) . . ?
O222 Cs1 O182 59.92(8) . 2_655 ?
O1W Cs1 O182 112.01(9) . 2_655 ?
O222 Cs1 Cl1 100.55(7) . 3_655 ?
O1W Cs1 Cl1 68.55(7) . 3_655 ?
O182 Cs1 Cl1 75.84(5) 2_655 3_655 ?
O222 Cs1 O92 134.49(8) . 1_455 ?
O1W Cs1 O92 90.80(8) . 1_455 ?
O182 Cs1 O92 157.03(7) 2_655 1_455 ?
Cl1 Cs1 O92 112.10(6) 3_655 1_455 ?
O222 Cs1 O122 63.35(8) . 2_655 ?
O1W Cs1 O122 72.39(8) . 2_655 ?
O182 Cs1 O122 116.96(7) 2_655 2_655 ?
Cl1 Cs1 O122 140.78(6) 3_655 2_655 ?
O92 Cs1 O122 71.35(8) 1_455 2_655 ?
O222 Cs1 O181 67.45(8) . 2_655 ?
O1W Cs1 O181 138.93(8) . 2_655 ?
O182 Cs1 O181 38.71(7) 2_655 2_655 ?
Cl1 Cs1 O181 111.75(5) 3_655 2_655 ?
O92 Cs1 O181 122.95(7) 1_455 2_655 ?
O122 Cs1 O181 95.28(7) 2_655 2_655 ?
O222 Cs1 O121 70.02(8) . 2_655 ?
O1W Cs1 O121 109.50(8) . 2_655 ?
O182 Cs1 O121 96.70(7) 2_655 2_655 ?
Cl1 Cs1 O121 170.25(5) 3_655 2_655 ?
O92 Cs1 O121 77.20(7) 1_455 2_655 ?
O122 Cs1 O121 37.67(7) 2_655 2_655 ?
O181 Cs1 O121 62.96(6) 2_655 2_655 ?
O222 Cs1 C18 55.73(9) . 2_655 ?
O1W Cs1 C18 121.67(9) . 2_655 ?
O182 Cs1 C18 19.55(8) 2_655 2_655 ?
Cl1 Cs1 C18 95.36(7) 3_655 2_655 ?
O92 Cs1 C18 144.02(8) 1_455 2_655 ?
O122 Cs1 C18 102.05(8) 2_655 2_655 ?
O181 Cs1 C18 21.08(8) 2_655 2_655 ?
O121 Cs1 C18 77.42(8) 2_655 2_655 ?
O222 Cs1 O72 130.25(8) . 4_565 ?
O1W Cs1 O72 132.27(9) . 4_565 ?
O182 Cs1 O72 70.33(7) 2_655 4_565 ?
Cl1 Cs1 O72 66.13(5) 3_655 4_565 ?
O92 Cs1 O72 92.66(7) 1_455 4_565 ?
O122 Cs1 O72 152.01(7) 2_655 4_565 ?
O181 Cs1 O72 73.86(7) 2_655 4_565 ?
O121 Cs1 O72 117.68(7) 2_655 4_565 ?
C18 Cs1 O72 77.18(8) 2_655 4_565 ?
O222 Cs1 C12 60.54(9) . 2_655 ?
O1W Cs1 C12 89.65(9) . 2_655 ?
O182 Cs1 C12 103.77(8) 2_655 2_655 ?
Cl1 Cs1 C12 155.47(7) 3_655 2_655 ?
O92 Cs1 C12 78.03(8) 1_455 2_655 ?
O122 Cs1 C12 18.93(8) 2_655 2_655 ?
O181 Cs1 C12 77.00(8) 2_655 2_655 ?
O121 Cs1 C12 19.89(8) 2_655 2_655 ?
C18 Cs1 C12 86.47(9) 2_655 2_655 ?
O72 Cs1 C12 137.52(8) 4_565 2_655 ?
O222 Cs1 C8 105.21(9) . 1_455 ?
O1W Cs1 C8 56.50(9) . 1_455 ?
O182 Cs1 C8 164.77(8) 2_655 1_455 ?
Cl1 Cs1 C8 105.75(7) 3_655 1_455 ?
O92 Cs1 C8 36.78(8) 1_455 1_455 ?
O122 Cs1 C8 52.34(8) 2_655 1_455 ?
O181 Cs1 C8 142.48(8) 2_655 1_455 ?
O121 Cs1 C8 79.79(8) 2_655 1_455 ?
C18 Cs1 C8 154.39(9) 2_655 1_455 ?
O72 Cs1 C8 124.48(8) 4_565 1_455 ?
C12 Cs1 C8 68.30(9) 2_655 1_455 ?
O222 Cs1 H1W1 66.7(10) . . ?
O1W Cs1 H1W1 12.6(6) . . ?
O182 Cs1 H1W1 99.9(6) 2_655 . ?
Cl1 Cs1 H1W1 60.4(9) 3_655 . ?
O92 Cs1 H1W1 102.7(7) 1_455 . ?
O122 Cs1 H1W1 80.5(9) 2_655 . ?
O181 Cs1 H1W1 130.3(8) 2_655 . ?
O121 Cs1 H1W1 115.8(9) 2_655 . ?
C18 Cs1 H1W1 111.2(7) 2_655 . ?
O72 Cs1 H1W1 126.3(9) 4_565 . ?
C12 Cs1 H1W1 96.1(9) 2_655 . ?
C8 Cs1 H1W1 69.0(6) 1_455 . ?
O182 Cs2 O202 160.15(8) 2_655 . ?
O182 Cs2 O2W 83.97(9) 2_655 . ?
O202 Cs2 O2W 81.53(9) . . ?
O182 Cs2 O1W 115.86(8) 2_655 3_655 ?
O202 Cs2 O1W 68.45(8) . 3_655 ?
O2W Cs2 O1W 138.11(9) . 3_655 ?
O182 Cs2 Cl1 122.36(6) 2_655 . ?
O202 Cs2 Cl1 77.42(6) . . ?
O2W Cs2 Cl1 135.82(7) . . ?
O1W Cs2 Cl1 65.97(7) 3_655 . ?
O182 Cs2 O12 92.11(7) 2_655 3_755 ?
O202 Cs2 O12 70.93(7) . 3_755 ?
O2W Cs2 O12 74.16(9) . 3_755 ?
O1W Cs2 O12 68.89(8) 3_655 3_755 ?
Cl1 Cs2 O12 131.73(5) . 3_755 ?
O182 Cs2 O222 55.71(8) 2_655 . ?
O202 Cs2 O222 137.14(7) . . ?
O2W Cs2 O222 89.21(8) . . ?
O1W Cs2 O222 132.65(8) 3_655 . ?
Cl1 Cs2 O222 80.86(6) . . ?
O12 Cs2 O222 145.60(7) 3_755 . ?
O182 Cs2 O221 76.21(7) 2_655 . ?
O202 Cs2 O221 107.75(7) . . ?
O2W Cs2 O221 60.37(8) . . ?
O1W Cs2 O221 155.90(8) 3_655 . ?
Cl1 Cs2 O221 89.93(5) . . ?
O12 Cs2 O221 133.79(7) 3_755 . ?
O222 Cs2 O221 35.62(7) . . ?
O182 Cs2 C20 154.39(9) 2_655 . ?
O202 Cs2 C20 18.34(8) . . ?
O2W Cs2 C20 70.47(9) . . ?
O1W Cs2 C20 85.62(9) 3_655 . ?
Cl1 Cs2 C20 77.95(7) . . ?
O12 Cs2 C20 82.56(8) 3_755 . ?
O222 Cs2 C20 120.49(8) . . ?
O221 Cs2 C20 89.45(8) . . ?
O182 Cs2 O201 134.61(7) 2_655 . ?
O202 Cs2 O201 36.32(7) . . ?
O2W Cs2 O201 51.42(8) . . ?
O1W Cs2 O201 104.77(8) 3_655 . ?
Cl1 Cs2 O201 91.52(5) . . ?
O12 Cs2 O201 84.04(7) 3_755 . ?
O222 Cs2 O201 109.09(7) . . ?
O221 Cs2 O201 74.50(6) . . ?
C20 Cs2 O201 20.12(8) . . ?
O182 Cs2 Cl1 72.52(6) 2_655 3_655 ?
O202 Cs2 Cl1 119.05(6) . 3_655 ?
O2W Cs2 Cl1 155.21(7) . 3_655 ?
O1W Cs2 Cl1 52.64(6) 3_655 3_655 ?
Cl1 Cs2 Cl1 66.54(3) . 3_655 ?
O12 Cs2 Cl1 98.47(5) 3_755 3_655 ?
O222 Cs2 Cl1 84.06(5) . 3_655 ?
O221 Cs2 Cl1 119.09(5) . 3_655 ?
C20 Cs2 Cl1 132.98(7) . 3_655 ?
O201 Cs2 Cl1 152.82(5) . 3_655 ?
O182 Cs2 C22 70.75(8) 2_655 . ?
O202 Cs2 C22 119.33(8) . . ?
O2W Cs2 C22 79.41(9) . . ?
O1W Cs2 C22 140.66(9) 3_655 . ?
Cl1 Cs2 C22 77.89(7) . . ?
O12 Cs2 C22 149.88(8) 3_755 . ?
O222 Cs2 C22 18.59(8) . . ?
O221 Cs2 C22 19.86(8) . . ?
C20 Cs2 C22 102.10(9) . . ?
O201 Cs2 C22 90.72(8) . . ?
Cl1 Cs2 C22 99.54(7) 3_655 . ?
O201 Zr1 O11 89.71(11) . . ?
O201 Zr1 O4 124.53(11) . . ?
O11 Zr1 O4 139.28(11) . . ?
O201 Zr1 O121 139.57(11) . . ?
O11 Zr1 O121 80.63(11) . . ?
O4 Zr1 O121 84.32(11) . . ?
O201 Zr1 O15 83.98(11) . . ?
O11 Zr1 O15 146.91(11) . . ?
O4 Zr1 O15 66.59(10) . . ?
O121 Zr1 O15 83.36(10) . . ?
O201 Zr1 O91 72.42(11) . . ?
O11 Zr1 O91 94.41(11) . . ?
O4 Zr1 O91 78.39(10) . . ?
O121 Zr1 O91 146.97(11) . . ?
O15 Zr1 O91 114.25(10) . . ?
O201 Zr1 N3 69.99(11) . . ?
O11 Zr1 N3 75.41(11) . . ?
O4 Zr1 N3 132.95(11) . . ?
O121 Zr1 N3 69.58(11) . . ?
O15 Zr1 N3 71.90(10) . . ?
O91 Zr1 N3 140.97(11) . . ?
O201 Zr1 N1 134.72(11) . . ?
O11 Zr1 N1 68.72(11) . . ?
O4 Zr1 N1 71.17(10) . . ?
O121 Zr1 N1 77.57(11) . . ?
O15 Zr1 N1 134.97(11) . . ?
O91 Zr1 N1 70.31(11) . . ?
N3 Zr1 N1 134.46(11) . . ?
O201 Zr1 Zr2 100.25(8) . . ?
O11 Zr1 Zr2 169.61(8) . . ?
O4 Zr1 Zr2 34.31(7) . . ?
O121 Zr1 Zr2 89.78(7) . . ?
O15 Zr1 Zr2 33.63(7) . . ?
O91 Zr1 Zr2 91.45(7) . . ?
N3 Zr1 Zr2 105.09(8) . . ?
N1 Zr1 Zr2 105.43(8) . . ?
O181 Zr2 O15 86.98(11) . . ?
O181 Zr2 O221 139.08(11) . . ?
O15 Zr2 O221 85.61(11) . . ?
O181 Zr2 O71 83.15(11) . . ?
O15 Zr2 O71 149.91(11) . . ?
O221 Zr2 O71 83.49(11) . . ?
O181 Zr2 O4 82.81(10) . . ?
O15 Zr2 O4 66.59(10) . . ?
O221 Zr2 O4 129.54(11) . . ?
O71 Zr2 O4 139.30(11) . . ?
O181 Zr2 O111 147.57(11) . . ?
O15 Zr2 O111 108.21(10) . . ?
O221 Zr2 O111 72.11(11) . . ?
O71 Zr2 O111 94.94(11) . . ?
O4 Zr2 O111 77.72(10) . . ?
O181 Zr2 N2 77.83(11) . . ?
O15 Zr2 N2 135.75(11) . . ?
O221 Zr2 N2 131.63(11) . . ?
O71 Zr2 N2 69.38(11) . . ?
O4 Zr2 N2 70.38(10) . . ?
O111 Zr2 N2 71.32(11) . . ?
O181 Zr2 N4 70.34(11) . . ?
O15 Zr2 N4 73.14(11) . . ?
O221 Zr2 N4 68.98(11) . . ?
O71 Zr2 N4 76.77(11) . . ?
O4 Zr2 N4 132.30(11) . . ?
O111 Zr2 N4 140.86(11) . . ?
N2 Zr2 N4 135.67(11) . . ?
O181 Zr2 Zr1 91.03(7) . . ?
O15 Zr2 Zr1 34.16(7) . . ?
O221 Zr2 Zr1 104.45(8) . . ?
O71 Zr2 Zr1 172.03(8) . . ?
O4 Zr2 Zr1 33.78(7) . . ?
O111 Zr2 Zr1 87.04(7) . . ?
N2 Zr2 Zr1 104.13(8) . . ?
N4 Zr2 Zr1 106.44(8) . . ?
C2 N1 C3 113.0(3) . . ?
C2 N1 C8 108.6(3) . . ?
C3 N1 C8 111.0(3) . . ?
C2 N1 Zr1 107.0(2) . . ?
C3 N1 Zr1 107.8(2) . . ?
C8 N1 Zr1 109.2(2) . . ?
O12 C1 O11 124.1(4) . . ?
O12 C1 C2 119.8(4) . . ?
O11 C1 C2 116.0(4) . . ?
N1 C2 C1 108.4(3) . . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C5 N2 C6 110.5(3) . . ?
C5 N2 C10 110.8(3) . . ?
C6 N2 C10 108.9(3) . . ?
C5 N2 Zr2 109.0(2) . . ?
C6 N2 Zr2 107.6(2) . . ?
C10 N2 Zr2 109.9(2) . . ?
N1 C3 C4 108.8(3) . . ?
N1 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
N1 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
C13 N3 C19 113.1(3) . . ?
C13 N3 C14 111.7(3) . . ?
C19 N3 C14 107.8(3) . . ?
C13 N3 Zr1 108.1(2) . . ?
C19 N3 Zr1 106.4(2) . . ?
C14 N3 Zr1 109.6(2) . . ?
C4 O4 Zr1 123.3(2) . . ?
C4 O4 Zr2 124.3(2) . . ?
Zr1 O4 Zr2 111.91(12) . . ?
C17 N4 C21 112.9(3) . . ?
C17 N4 C16 112.1(3) . . ?
C21 N4 C16 108.0(3) . . ?
C17 N4 Zr2 109.3(2) . . ?
C21 N4 Zr2 106.8(2) . . ?
C16 N4 Zr2 107.5(2) . . ?
O4 C4 C3 107.1(3) . . ?
O4 C4 C5 107.2(3) . . ?
C3 C4 C5 112.2(3) . . ?
O4 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C5 C4 H4A 110.1 . . ?
N2 C5 C4 108.5(3) . . ?
N2 C5 H5A 110.0 . . ?
C4 C5 H5A 110.0 . . ?
N2 C5 H5B 110.0 . . ?
C4 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N2 C6 C7 110.0(3) . . ?
N2 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
O72 C7 O71 124.8(4) . . ?
O72 C7 C6 119.5(4) . . ?
O71 C7 C6 115.7(3) . . ?
N1 C8 C9 112.0(3) . . ?
N1 C8 Cs1 162.3(3) . 1_655 ?
C9 C8 Cs1 85.6(2) . 1_655 ?
N1 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
Cs1 C8 H8A 61.1 1_655 . ?
N1 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
Cs1 C8 H8B 63.9 1_655 . ?
H8A C8 H8B 107.9 . . ?
O92 C9 O91 125.7(4) . . ?
O92 C9 C8 117.7(4) . . ?
O91 C9 C8 116.6(4) . . ?
N2 C10 C11 112.4(3) . . ?
N2 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
N2 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
C1 O11 Zr1 124.7(3) . . ?
O112 C11 O111 123.9(4) . . ?
O112 C11 C10 119.4(4) . . ?
O111 C11 C10 116.7(4) . . ?
C1 O12 Cs2 109.4(3) . 3_755 ?
O122 C12 O121 123.7(4) . . ?
O122 C12 C13 119.2(4) . . ?
O121 C12 C13 117.0(4) . . ?
O122 C12 Cs1 63.7(2) . 2_645 ?
O121 C12 Cs1 66.7(2) . 2_645 ?
C13 C12 Cs1 155.4(3) . 2_645 ?
N3 C13 C12 110.6(3) . . ?
N3 C13 H13A 109.5 . . ?
C12 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
N3 C14 C15 110.4(3) . . ?
N3 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
N3 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C15 O15 Zr2 118.7(2) . . ?
C15 O15 Zr1 118.7(2) . . ?
Zr2 O15 Zr1 112.20(12) . . ?
O15 C15 C16 107.7(3) . . ?
O15 C15 C14 107.2(3) . . ?
C16 C15 C14 111.8(3) . . ?
O15 C15 H15A 110.0 . . ?
C16 C15 H15A 110.0 . . ?
C14 C15 H15A 110.0 . . ?
N4 C16 C15 110.9(3) . . ?
N4 C16 H16A 109.5 . . ?
C15 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.0 . . ?
N4 C17 C18 112.0(3) . . ?
N4 C17 H17A 109.2 . . ?
C18 C17 H17A 109.2 . . ?
N4 C17 H17B 109.2 . . ?
C18 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
O182 C18 O181 124.1(4) . . ?
O182 C18 C17 120.0(4) . . ?
O181 C18 C17 115.8(4) . . ?
O182 C18 Cs1 63.1(2) . 2_645 ?
O181 C18 Cs1 72.3(2) . 2_645 ?
C17 C18 Cs1 144.9(3) . 2_645 ?
N3 C19 C20 106.3(3) . . ?
N3 C19 H19A 110.5 . . ?
C20 C19 H19A 110.5 . . ?
N3 C19 H19B 110.5 . . ?
C20 C19 H19B 110.5 . . ?
H19A C19 H19B 108.7 . . ?
O202 C20 O201 125.0(4) . . ?
O202 C20 C19 121.4(4) . . ?
O201 C20 C19 113.6(3) . . ?
O202 C20 Cs2 52.3(2) . . ?
O201 C20 Cs2 85.3(2) . . ?
C19 C20 Cs2 138.6(3) . . ?
N4 C21 C22 109.8(3) . . ?
N4 C21 H21A 109.7 . . ?
C22 C21 H21A 109.7 . . ?
N4 C21 H21B 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
O222 C22 O221 124.4(4) . . ?
O222 C22 C21 120.8(4) . . ?
O221 C22 C21 114.8(4) . . ?
O222 C22 Cs2 71.6(3) . . ?
O221 C22 Cs2 72.9(2) . . ?
C21 C22 Cs2 132.0(3) . . ?
C7 O71 Zr2 123.3(3) . . ?
C7 O72 Cs1 124.9(3) . 4_666 ?
C9 O91 Zr1 125.7(3) . . ?
C9 O92 Cs1 114.3(3) . 1_655 ?
C9 O92 H3W4 127(3) . . ?
Cs1 O92 H3W4 108(3) 1_655 . ?
C11 O111 Zr2 125.1(3) . . ?
C12 O121 Zr1 123.1(3) . . ?
C12 O121 Cs1 93.4(2) . 2_645 ?
Zr1 O121 Cs1 142.27(11) . 2_645 ?
C12 O122 Cs1 97.4(3) . 2_645 ?
C18 O181 Zr2 125.0(3) . . ?
C18 O181 Cs1 86.6(2) . 2_645 ?
Zr2 O181 Cs1 145.40(11) . 2_645 ?
C18 O182 Cs2 132.8(3) . 2_645 ?
C18 O182 Cs1 97.4(3) . 2_645 ?
Cs2 O182 Cs1 96.53(8) 2_645 2_645 ?
C20 O201 Zr1 126.1(3) . . ?
C20 O201 Cs2 74.6(2) . . ?
Zr1 O201 Cs2 130.28(11) . . ?
C20 O202 Cs2 109.3(3) . . ?
C22 O221 Zr2 125.7(3) . . ?
C22 O221 Cs2 87.2(2) . . ?
Zr2 O221 Cs2 129.28(11) . . ?
C22 O222 Cs1 162.8(3) . . ?
C22 O222 Cs2 89.8(3) . . ?
Cs1 O222 Cs2 88.85(8) . . ?
Cs1 Cl1 Cs2 100.36(3) 3_655 . ?
Cs1 Cl1 Cs2 81.40(2) 3_655 3_655 ?
Cs2 Cl1 Cs2 113.46(3) . 3_655 ?
Cs1 O1W Cs2 110.06(11) . 3_655 ?
Cs1 O1W H1W1 108(5) . . ?
Cs2 O1W H1W1 74(5) 3_655 . ?
Cs1 O1W H2W1 128(5) . . ?
Cs2 O1W H2W1 121(5) 3_655 . ?
H1W1 O1W H2W1 98(6) . . ?
Cs2 O2W H1W2 100(4) . . ?
Cs2 O2W H2W2 106(6) . . ?
H1W2 O2W H2W2 113(7) . . ?
H1W3 O3W H2W3 107(7) . . ?
H1W3 O3W H2W4 101(6) . . ?
H2W3 O3W H2W4 132(5) . . ?
H1W4 O4W H2W4 109(5) . . ?
H1W4 O4W H3W4 108(6) . . ?
H2W4 O4W H3W4 114(5) . . ?
H1W5 O5W H2W5 100(6) . . ?
H1W6 O6W H2W6 109(7) . . ?
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
Cs1 O222 3.049(3) . ?
Cs1 O1W 3.086(4) . ?
Cs1 O182 3.241(3) 2_655 ?
Cs1 Cl1 3.3834(12) 3_655 ?
Cs1 O92 3.416(3) 1_455 ?
Cs1 O122 3.421(3) 2_655 ?
Cs1 O181 3.441(3) 2_655 ?
Cs1 O121 3.482(3) 2_655 ?
Cs1 C18 3.606(4) 2_655 ?
Cs1 O72 3.625(3) 4_565 ?
Cs1 C12 3.784(4) 2_655 ?
Cs1 C8 3.918(4) 1_455 ?
Cs1 H1W1 3.41(5) . ?
Cs2 O182 3.029(3) 2_655 ?
Cs2 O202 3.066(3) . ?
Cs2 O2W 3.275(4) . ?
Cs2 O1W 3.287(4) 3_655 ?
Cs2 Cl1 3.4174(12) . ?
Cs2 O12 3.534(4) 3_755 ?
Cs2 O222 3.614(3) . ?
Cs2 O221 3.645(3) . ?
Cs2 C20 3.656(4) . ?
Cs2 O201 3.778(3) . ?
Cs2 Cl1 3.7806(12) 3_655 ?
Cs2 C22 3.809(4) . ?
Zr1 O201 2.116(3) . ?
Zr1 O11 2.140(3) . ?
Zr1 O4 2.146(3) . ?
Zr1 O121 2.169(3) . ?
Zr1 O15 2.172(3) . ?
Zr1 O91 2.202(3) . ?
Zr1 N3 2.446(3) . ?
Zr1 N1 2.453(3) . ?
Zr1 Zr2 3.5807(5) . ?
Zr2 O181 2.127(3) . ?
Zr2 O15 2.142(3) . ?
Zr2 O221 2.146(3) . ?
Zr2 O71 2.166(3) . ?
Zr2 O4 2.176(3) . ?
Zr2 O111 2.187(3) . ?
Zr2 N2 2.429(3) . ?
Zr2 N4 2.454(3) . ?
N1 C2 1.479(5) . ?
N1 C3 1.483(5) . ?
N1 C8 1.486(5) . ?
C1 O12 1.232(5) . ?
C1 O11 1.288(5) . ?
C1 C2 1.519(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N2 C5 1.480(5) . ?
N2 C6 1.483(5) . ?
N2 C10 1.488(5) . ?
C3 C4 1.516(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N3 C13 1.478(5) . ?
N3 C19 1.479(5) . ?
N3 C14 1.504(5) . ?
O4 C4 1.420(5) . ?
N4 C17 1.479(5) . ?
N4 C21 1.485(5) . ?
N4 C16 1.491(5) . ?
C4 C5 1.520(5) . ?
C4 H4A 1.0000 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.520(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O72 1.227(5) . ?
C7 O71 1.298(5) . ?
C8 C9 1.508(6) . ?
C8 Cs1 3.918(4) 1_655 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 O92 1.248(5) . ?
C9 O91 1.267(5) . ?
C10 C11 1.511(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 O112 1.236(5) . ?
C11 O111 1.282(5) . ?
O12 Cs2 3.534(4) 3_755 ?
C12 O122 1.238(5) . ?
C12 O121 1.290(5) . ?
C12 C13 1.512(6) . ?
C12 Cs1 3.784(4) 2_645 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.511(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O15 C15 1.431(5) . ?
C15 C16 1.510(5) . ?
C15 H15A 1.0000 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.523(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 O182 1.216(5) . ?
C18 O181 1.299(5) . ?
C18 Cs1 3.606(4) 2_645 ?
C19 C20 1.532(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 O202 1.219(5) . ?
C20 O201 1.304(5) . ?
C21 C22 1.514(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 O222 1.215(5) . ?
C22 O221 1.295(5) . ?
O72 Cs1 3.625(3) 4_666 ?
O92 Cs1 3.416(3) 1_655 ?
O92 H3W4 1.41(9) . ?
O121 Cs1 3.482(3) 2_645 ?
O122 Cs1 3.421(3) 2_645 ?
O181 Cs1 3.441(3) 2_645 ?
O182 Cs2 3.029(3) 2_645 ?
O182 Cs1 3.241(3) 2_645 ?
Cl1 Cs1 3.3834(12) 3_655 ?
Cl1 Cs2 3.7806(12) 3_655 ?
O1W Cs2 3.287(4) 3_655 ?
O1W H1W1 0.78(2) . ?
O1W H2W1 0.78(2) . ?
O2W H1W2 0.78(2) . ?
O2W H2W2 0.78(2) . ?
O3W H1W3 0.78(2) . ?
O3W H2W3 0.78(2) . ?
O3W H2W4 1.39(5) . ?
O4W H1W4 0.78(2) . ?
O4W H2W4 1.10(5) . ?
O4W H3W4 1.13(9) . ?
O5W H1W5 0.78(2) . ?
O5W H2W5 0.78(2) . ?
O6W H1W6 0.78(2) . ?
O6W H2W6 0.78(2) . ?
