# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Zr[(PDC)2(H2O)2](H2O)1.3
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C14 H12.6 N2 O11.3 Zr'
_chemical_formula_weight         477.60

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_cell_length_a                   23.7011(7)
_cell_length_b                   12.1758(3)
_cell_length_c                   14.3519(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.526(2)
_cell_angle_gamma                90
_cell_volume                     3990.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    173.0(2)

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904.6
_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.014
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
; 
 SADABS(Blessing, 1995) 
;
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  0.99

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      173.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_number            27544
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             3516
_reflns_number_gt                2661
_reflns_threshold_expression     >2sĬ)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0616P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3516
_refine_ls_number_parameters     269
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1602
_refine_ls_wR_factor_gt          0.1534
_refine_ls_goodness_of_fit_ref   1.454
_refine_ls_restrained_S_all      1.548
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.129

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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
Zr1 Zr 0.15408(2) 0.13398(4) 0.21232(4) 0.0161(2) Uani 1 1 d . . .
OW1 O 0.24877(18) 0.1381(3) 0.2693(3) 0.0252(10) Uani 1 1 d D . .
H100 H 0.2619 0.0756 0.2705 0.038 Uiso 1 1 calc RD . .
H101 H 0.273(3) 0.190(4) 0.279(5) 0.06(3) Uiso 1 1 d D . .
OW2 O 0.1562(2) 0.1020(4) 0.0635(3) 0.0277(11) Uani 1 1 d D . .
H200 H 0.159(3) 0.0321(18) 0.0550(13) 0.041 Uiso 1 1 calc RD . .
H201 H 0.157(4) 0.151(6) 0.019(5) 0.10(4) Uiso 1 1 d D . .
O3 O 0.18704(17) -0.0367(3) 0.2209(3) 0.0210(10) Uani 1 1 d . . .
O4 O 0.17145(19) -0.2171(3) 0.2306(3) 0.0324(11) Uani 1 1 d . . .
O5 O 0.07097(17) 0.2132(3) 0.1711(3) 0.0244(10) Uani 1 1 d . . .
O6 O -0.02667(19) 0.2138(4) 0.1212(3) 0.0405(13) Uani 1 1 d . . .
O7 O 0.17644(17) 0.2883(3) 0.1516(3) 0.0209(10) Uani 1 1 d . . .
O8 O 0.18538(19) 0.4696(3) 0.1551(3) 0.0276(11) Uani 1 1 d . . .
O9 O 0.14606(17) 0.0780(3) 0.3515(3) 0.0209(10) Uani 1 1 d . . .
O10 O 0.15366(19) 0.1033(3) 0.5083(3) 0.0283(11) Uani 1 1 d . . .
N1 N 0.0790(2) 0.0076(4) 0.1686(3) 0.0197(12) Uani 1 1 d . . .
N2 N 0.1678(2) 0.2746(4) 0.3232(3) 0.0178(11) Uani 1 1 d . . .
C1 C 0.0909(3) -0.0998(5) 0.1738(4) 0.0191(14) Uani 1 1 d . . .
C2 C 0.0463(3) -0.1753(5) 0.1479(5) 0.0295(16) Uani 1 1 d . . .
H2 H 0.0546 -0.25 0.1519 0.035 Uiso 1 1 calc R . .
C3 C -0.0107(3) -0.1400(5) 0.1160(5) 0.0341(17) Uani 1 1 d . . .
H3 H -0.0411 -0.1903 0.0965 0.041 Uiso 1 1 calc R . .
C4 C -0.0221(3) -0.0291(5) 0.1133(5) 0.0311(16) Uani 1 1 d . . .
H4 H -0.0605 -0.0038 0.0933 0.037 Uiso 1 1 calc R . .
C5 C 0.0235(3) 0.0438(5) 0.1404(4) 0.0251(15) Uani 1 1 d . . .
C6 C 0.1541(3) -0.1206(5) 0.2096(4) 0.0217(15) Uani 1 1 d . . .
C7 C 0.0199(3) 0.1670(5) 0.1431(4) 0.0248(15) Uani 1 1 d . . .
C8 C 0.1789(3) 0.3758(5) 0.2968(4) 0.0201(14) Uani 1 1 d . . .
C9 C 0.1881(3) 0.4618(5) 0.3606(5) 0.0367(18) Uani 1 1 d . . .
H9 H 0.1959 0.5318 0.3413 0.044 Uiso 1 1 calc R . .
C10 C 0.1855(4) 0.4421(6) 0.4564(5) 0.044(2) Uani 1 1 d . . .
H10 H 0.1914 0.4987 0.5014 0.053 Uiso 1 1 calc R . .
C11 C 0.1740(3) 0.3356(5) 0.4814(5) 0.0350(18) Uani 1 1 d . . .
H11 H 0.1722 0.3199 0.544 0.042 Uiso 1 1 calc R . .
C12 C 0.1653(3) 0.2539(5) 0.4131(4) 0.0206(14) Uani 1 1 d . . .
C13 C 0.1806(3) 0.3811(5) 0.1932(4) 0.0189(14) Uani 1 1 d . . .
C14 C 0.1538(3) 0.1361(5) 0.4273(4) 0.0184(14) Uani 1 1 d . . .
OW3 O -0.0785(6) -0.3828(8) 0.0446(7) 0.084(3) Uani 0.547(8) 1 d P . .
OW4 O 0.1888(4) 0.2385(6) -0.0573(5) 0.084(3) Uani 0.712(9) 1 d P . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Zr1 O5 2.130(4) . ?
Zr1 O9 2.166(4) . ?
Zr1 OW1 2.174(4) . ?
Zr1 OW2 2.184(4) . ?
Zr1 O7 2.195(4) . ?
Zr1 O3 2.212(4) . ?
Zr1 N2 2.301(4) . ?
Zr1 N1 2.309(5) . ?
O3 C6 1.270(7) . ?
O4 C6 1.254(7) . ?
O5 C7 1.296(7) . ?
O6 C7 1.208(7) . ?
O7 C13 1.270(6) . ?
O8 C13 1.227(6) . ?
O9 C14 1.270(7) . ?
O10 C14 1.229(7) . ?
N1 C1 1.337(7) . ?
N1 C5 1.343(7) . ?
N2 C12 1.330(7) . ?
N2 C8 1.337(7) . ?
C1 C2 1.374(8) . ?
C1 C6 1.469(8) . ?
C2 C3 1.372(9) . ?
C3 C4 1.376(8) . ?
C4 C5 1.372(9) . ?
C5 C7 1.504(9) . ?
C8 C9 1.369(8) . ?
C8 C13 1.500(8) . ?
C9 C10 1.412(9) . ?
C10 C11 1.392(9) . ?
C11 C12 1.373(8) . ?
C12 C14 1.484(8) . ?

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
O5 Zr1 O9 95.50(15) . . ?
O5 Zr1 OW1 151.52(15) . . ?
O9 Zr1 OW1 89.84(15) . . ?
O5 Zr1 OW2 94.04(16) . . ?
O9 Zr1 OW2 151.16(17) . . ?
OW1 Zr1 OW2 94.60(17) . . ?
O5 Zr1 O7 78.81(15) . . ?
O9 Zr1 O7 136.52(14) . . ?
OW1 Zr1 O7 78.15(15) . . ?
OW2 Zr1 O7 72.11(15) . . ?
O5 Zr1 O3 136.66(15) . . ?
O9 Zr1 O3 76.72(15) . . ?
OW1 Zr1 O3 71.78(14) . . ?
OW2 Zr1 O3 77.68(16) . . ?
O7 Zr1 O3 134.98(15) . . ?
O5 Zr1 N2 78.70(16) . . ?
O9 Zr1 N2 68.10(15) . . ?
OW1 Zr1 N2 77.44(16) . . ?
OW2 Zr1 N2 140.63(17) . . ?
O7 Zr1 N2 68.52(15) . . ?
O3 Zr1 N2 132.72(15) . . ?
O5 Zr1 N1 68.76(16) . . ?
O9 Zr1 N1 77.85(15) . . ?
OW1 Zr1 N1 139.55(16) . . ?
OW2 Zr1 N1 80.41(16) . . ?
O7 Zr1 N1 135.46(15) . . ?
O3 Zr1 N1 67.93(15) . . ?
N2 Zr1 N1 129.75(16) . . ?
C6 O3 Zr1 123.5(4) . . ?
C7 O5 Zr1 127.4(4) . . ?
C13 O7 Zr1 124.8(4) . . ?
C14 O9 Zr1 126.0(4) . . ?
C1 N1 C5 120.9(5) . . ?
C1 N1 Zr1 120.1(4) . . ?
C5 N1 Zr1 119.0(4) . . ?
C12 N2 C8 120.8(5) . . ?
C12 N2 Zr1 119.7(4) . . ?
C8 N2 Zr1 119.5(4) . . ?
N1 C1 C2 120.2(6) . . ?
N1 C1 C6 111.6(5) . . ?
C2 C1 C6 128.2(6) . . ?
C1 C2 C3 119.8(6) . . ?
C2 C3 C4 119.1(6) . . ?
C5 C4 C3 119.5(6) . . ?
N1 C5 C4 120.5(6) . . ?
N1 C5 C7 112.1(5) . . ?
C4 C5 C7 127.4(6) . . ?
O4 C6 O3 124.8(6) . . ?
O4 C6 C1 118.9(5) . . ?
O3 C6 C1 116.2(5) . . ?
O6 C7 O5 126.1(6) . . ?
O6 C7 C5 121.2(6) . . ?
O5 C7 C5 112.8(5) . . ?
N2 C8 C9 121.6(6) . . ?
N2 C8 C13 112.4(5) . . ?
C9 C8 C13 126.0(5) . . ?
C8 C9 C10 118.7(6) . . ?
C11 C10 C9 118.2(6) . . ?
C12 C11 C10 119.5(6) . . ?
N2 C12 C11 121.2(6) . . ?
N2 C12 C14 111.9(5) . . ?
C11 C12 C14 126.8(5) . . ?
O8 C13 O7 125.2(5) . . ?
O8 C13 C8 120.7(5) . . ?
O7 C13 C8 114.1(5) . . ?
O10 C14 O9 126.4(5) . . ?
O10 C14 C12 119.4(5) . . ?
O9 C14 C12 114.2(5) . . ?
_database_code_depnum_ccdc_archive 'CCDC 971388'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Zr[(PDC)2(DMF)2](DMF)
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C23 H27 N5 O11 Zr'
_chemical_formula_weight         640.72

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_cell_length_a                   30.4402(13)
_cell_length_b                   11.6778(4)
_cell_length_c                   15.9518(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.695(3)
_cell_angle_gamma                90
_cell_volume                     5589.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173.0(2)

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2624
_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.047
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
; 
 SADABS(Blessing, 1995) 
;
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.98

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      173.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_av_unetI/netI     0.1593
_diffrn_reflns_number            47677
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_reflns_number_total             6889
_reflns_number_gt                3047
_reflns_threshold_expression     >2sĬ)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0444P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6889
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.0948
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   0.724
_refine_ls_restrained_S_all      0.724
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.51
_refine_diff_density_rms         0.08

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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
Zr1 Zr 0.400004(10) 0.76661(2) 0.03284(2) 0.03214(12) Uani 1 1 d . . .
O1 O 0.34801(6) 0.89964(17) 0.01047(13) 0.0402(6) Uani 1 1 d . . .
O2 O 0.32572(7) 1.08147(19) 0.01415(15) 0.0551(7) Uani 1 1 d . . .
O3 O 0.47019(7) 0.75943(17) 0.07104(14) 0.0432(6) Uani 1 1 d . . .
O4 O 0.53675(8) 0.8379(2) 0.11975(18) 0.0784(9) Uani 1 1 d . . .
O5 O 0.40488(7) 0.82411(17) -0.09198(14) 0.0426(6) Uani 1 1 d . . .
O6 O 0.41970(9) 0.79885(19) -0.22324(15) 0.0615(7) Uani 1 1 d . . .
O7 O 0.40677(7) 0.60511(17) 0.10249(13) 0.0411(6) Uani 1 1 d . . .
O8 O 0.42708(9) 0.4212(2) 0.11504(15) 0.0684(8) Uani 1 1 d . . .
O9 O 0.38618(7) 0.80856(18) 0.15910(15) 0.0457(6) Uani 1 1 d . . .
O10 O 0.33813(7) 0.67514(18) -0.01749(15) 0.0475(6) Uani 1 1 d . . .
N1 N 0.42928(9) 0.9464(2) 0.06355(15) 0.0329(7) Uani 1 1 d . . .
N2 N 0.42301(8) 0.6212(2) -0.04757(16) 0.0322(6) Uani 1 1 d . . .
N3 N 0.36771(8) 0.8096(2) 0.28924(18) 0.0412(7) Uani 1 1 d . . .
N4 N 0.27075(9) 0.6296(3) -0.08992(19) 0.0520(8) Uani 1 1 d . . .
C1 C 0.40222(11) 1.0375(3) 0.05867(19) 0.0324(8) Uani 1 1 d . . .
C2 C 0.41868(11) 1.1439(3) 0.0844(2) 0.0397(9) Uani 1 1 d . . .
H2 H 0.4 1.2074 0.0802 0.048 Uiso 1 1 calc R . .
C3 C 0.46341(12) 1.1547(3) 0.1167(2) 0.0460(9) Uani 1 1 d . . .
H3 H 0.475 1.2258 0.1353 0.055 Uiso 1 1 calc R . .
C4 C 0.49100(11) 1.0610(3) 0.1215(2) 0.0446(9) Uani 1 1 d . . .
H4 H 0.5213 1.0673 0.1426 0.053 Uiso 1 1 calc R . .
C5 C 0.47229(11) 0.9575(3) 0.0941(2) 0.0362(8) Uani 1 1 d . . .
C6 C 0.35450(11) 1.0078(3) 0.0252(2) 0.0379(8) Uani 1 1 d . . .
C7 C 0.49663(12) 0.8447(3) 0.0965(2) 0.0469(10) Uani 1 1 d . . .
C8 C 0.42967(10) 0.6436(3) -0.1263(2) 0.0346(8) Uani 1 1 d . . .
C9 C 0.44669(11) 0.5617(3) -0.1748(2) 0.0451(9) Uani 1 1 d . . .
H9 H 0.4508 0.5774 -0.2301 0.054 Uiso 1 1 calc R . .
C10 C 0.45745(12) 0.4557(3) -0.1383(2) 0.0521(10) Uani 1 1 d . . .
H10 H 0.4695 0.3993 -0.1688 0.063 Uiso 1 1 calc R . .
C11 C 0.45036(11) 0.4337(3) -0.0569(2) 0.0465(9) Uani 1 1 d . . .
H11 H 0.4574 0.3624 -0.0322 0.056 Uiso 1 1 calc R . .
C12 C 0.43258(10) 0.5186(3) -0.0121(2) 0.0336(8) Uani 1 1 d . . .
C13 C 0.41747(11) 0.7644(3) -0.1527(2) 0.0391(8) Uani 1 1 d . . .
C14 C 0.42196(11) 0.5111(3) 0.0755(2) 0.0403(9) Uani 1 1 d . . .
C15 C 0.35800(13) 0.7451(3) 0.3623(2) 0.0743(13) Uani 1 1 d . . .
H15A H 0.3584 0.6647 0.3501 0.111 Uiso 1 1 calc R . .
H15B H 0.3291 0.7664 0.3737 0.111 Uiso 1 1 calc R . .
H15C H 0.3801 0.7619 0.4111 0.111 Uiso 1 1 calc R . .
C16 C 0.36947(11) 0.9338(3) 0.2969(2) 0.0588(11) Uani 1 1 d . . .
H16A H 0.3762 0.9664 0.2452 0.088 Uiso 1 1 calc R . .
H16B H 0.3922 0.955 0.3435 0.088 Uiso 1 1 calc R . .
H16C H 0.3412 0.9619 0.3069 0.088 Uiso 1 1 calc R . .
C17 C 0.37697(11) 0.7570(3) 0.2227(2) 0.0409(9) Uani 1 1 d . . .
C18 C 0.27600(13) 0.5087(3) -0.0688(3) 0.0891(15) Uani 1 1 d . . .
H18A H 0.2777 0.4656 -0.1194 0.134 Uiso 1 1 calc R . .
H18B H 0.2509 0.483 -0.0445 0.134 Uiso 1 1 calc R . .
H18C H 0.3029 0.4977 -0.0285 0.134 Uiso 1 1 calc R . .
C19 C 0.22930(12) 0.6651(4) -0.1435(3) 0.0816(14) Uani 1 1 d . . .
H19A H 0.2046 0.6469 -0.1157 0.122 Uiso 1 1 calc R . .
H19B H 0.2261 0.6257 -0.197 0.122 Uiso 1 1 calc R . .
H19C H 0.23 0.7462 -0.1531 0.122 Uiso 1 1 calc R . .
C20 C 0.30239(13) 0.7026(3) -0.0633(2) 0.0470(10) Uani 1 1 d . . .
O11 O 0.27152(18) 0.4326(4) 0.7046(3) 0.176(2) Uani 1 1 d . . .
N5 N 0.29101(13) 0.6073(3) 0.6654(2) 0.0739(10) Uani 1 1 d . . .
C21 C 0.2789(2) 0.7032(5) 0.6140(4) 0.170(3) Uani 1 1 d . . .
H21A H 0.2479 0.6989 0.5902 0.255 Uiso 1 1 calc R . .
H21B H 0.2963 0.7051 0.569 0.255 Uiso 1 1 calc R . .
H21C H 0.2845 0.7715 0.6477 0.255 Uiso 1 1 calc R . .
C22 C 0.33193(16) 0.5992(5) 0.7192(3) 0.143(2) Uani 1 1 d . . .
H22A H 0.3356 0.6635 0.7572 0.214 Uiso 1 1 calc R . .
H22B H 0.3555 0.5988 0.686 0.214 Uiso 1 1 calc R . .
H22C H 0.3329 0.5296 0.7515 0.214 Uiso 1 1 calc R . .
C23 C 0.26241(19) 0.5183(6) 0.6594(4) 0.1088(18) Uani 1 1 d . . .
H23 H 0.2358 0.5213 0.6212 0.131 Uiso 1 1 calc R . .
H201 H 0.2965(10) 0.783(3) -0.084(2) 0.063(11) Uiso 1 1 d . . .
H171 H 0.3770(9) 0.678(3) 0.2235(18) 0.045(10) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Zr1 O3 2.122(2) . ?
Zr1 O5 2.130(2) . ?
Zr1 O7 2.181(2) . ?
Zr1 O9 2.182(2) . ?
Zr1 O10 2.196(2) . ?
Zr1 O1 2.204(2) . ?
Zr1 N1 2.301(2) . ?
Zr1 N2 2.307(2) . ?
O1 C6 1.293(3) . ?
O2 C6 1.220(3) . ?
O3 C7 1.302(4) . ?
O4 C7 1.218(3) . ?
O5 C13 1.302(4) . ?
O6 C13 1.208(3) . ?
O7 C14 1.293(3) . ?
O8 C14 1.221(4) . ?
O9 C17 1.252(4) . ?
O10 C20 1.246(4) . ?
N1 C5 1.324(3) . ?
N1 C1 1.340(3) . ?
N2 C12 1.336(3) . ?
N2 C8 1.331(4) . ?
N3 C17 1.298(4) . ?
N3 C16 1.455(4) . ?
N3 C15 1.458(4) . ?
N4 C20 1.303(4) . ?
N4 C18 1.454(4) . ?
N4 C19 1.460(4) . ?
C1 C2 1.377(4) . ?
C1 C6 1.502(4) . ?
C2 C3 1.378(4) . ?
C3 C4 1.374(4) . ?
C4 C5 1.376(4) . ?
C5 C7 1.508(4) . ?
C8 C9 1.385(4) . ?
C8 C13 1.500(4) . ?
C9 C10 1.383(4) . ?
C10 C11 1.376(4) . ?
C11 C12 1.384(4) . ?
C12 C14 1.489(4) . ?
O11 C23 1.238(6) . ?
N5 C23 1.349(6) . ?
N5 C22 1.392(5) . ?
N5 C21 1.400(5) . ?

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 Zr1 O5 93.19(8) . . ?
O3 Zr1 O7 79.36(8) . . ?
O5 Zr1 O7 137.17(8) . . ?
O3 Zr1 O9 94.88(8) . . ?
O5 Zr1 O9 147.87(8) . . ?
O7 Zr1 O9 74.94(8) . . ?
O3 Zr1 O10 147.74(8) . . ?
O5 Zr1 O10 90.12(8) . . ?
O7 Zr1 O10 76.54(8) . . ?
O9 Zr1 O10 99.20(8) . . ?
O3 Zr1 O1 137.33(8) . . ?
O5 Zr1 O1 77.74(8) . . ?
O7 Zr1 O1 134.09(8) . . ?
O9 Zr1 O1 75.30(8) . . ?
O10 Zr1 O1 74.65(8) . . ?
O3 Zr1 N1 68.89(8) . . ?
O5 Zr1 N1 79.97(8) . . ?
O7 Zr1 N1 132.89(8) . . ?
O9 Zr1 N1 74.13(8) . . ?
O10 Zr1 N1 143.04(9) . . ?
O1 Zr1 N1 68.47(8) . . ?
O3 Zr1 N2 75.25(8) . . ?
O5 Zr1 N2 68.70(8) . . ?
O7 Zr1 N2 68.61(8) . . ?
O9 Zr1 N2 143.37(9) . . ?
O10 Zr1 N2 76.16(8) . . ?
O1 Zr1 N2 134.91(8) . . ?
N1 Zr1 N2 130.32(9) . . ?
C6 O1 Zr1 125.1(2) . . ?
C7 O3 Zr1 126.8(2) . . ?
C13 O5 Zr1 127.0(2) . . ?
C14 O7 Zr1 125.0(2) . . ?
C17 O9 Zr1 138.1(2) . . ?
C20 O10 Zr1 134.4(2) . . ?
C5 N1 C1 120.3(3) . . ?
C5 N1 Zr1 119.4(2) . . ?
C1 N1 Zr1 120.0(2) . . ?
C12 N2 C8 121.3(3) . . ?
C12 N2 Zr1 119.3(2) . . ?
C8 N2 Zr1 119.23(19) . . ?
C17 N3 C16 122.0(3) . . ?
C17 N3 C15 120.6(3) . . ?
C16 N3 C15 117.2(3) . . ?
C20 N4 C18 120.9(3) . . ?
C20 N4 C19 121.6(3) . . ?
C18 N4 C19 117.5(3) . . ?
N1 C1 C2 120.7(3) . . ?
N1 C1 C6 112.7(3) . . ?
C2 C1 C6 126.6(3) . . ?
C1 C2 C3 118.8(3) . . ?
C4 C3 C2 120.3(3) . . ?
C3 C4 C5 117.8(3) . . ?
N1 C5 C4 122.2(3) . . ?
N1 C5 C7 112.1(3) . . ?
C4 C5 C7 125.7(3) . . ?
O2 C6 O1 125.4(3) . . ?
O2 C6 C1 121.1(3) . . ?
O1 C6 C1 113.5(3) . . ?
O4 C7 O3 125.5(3) . . ?
O4 C7 C5 121.9(3) . . ?
O3 C7 C5 112.6(3) . . ?
N2 C8 C9 121.4(3) . . ?
N2 C8 C13 112.3(3) . . ?
C9 C8 C13 126.2(3) . . ?
C10 C9 C8 117.9(3) . . ?
C9 C10 C11 120.0(3) . . ?
C12 C11 C10 119.4(3) . . ?
N2 C12 C11 120.0(3) . . ?
N2 C12 C14 112.6(3) . . ?
C11 C12 C14 127.4(3) . . ?
O6 C13 O5 125.7(3) . . ?
O6 C13 C8 121.7(3) . . ?
O5 C13 C8 112.6(3) . . ?
O8 C14 O7 125.4(3) . . ?
O8 C14 C12 120.4(3) . . ?
O7 C14 C12 114.1(3) . . ?
O9 C17 N3 122.9(4) . . ?
O10 C20 N4 123.2(4) . . ?
C23 N5 C22 119.4(5) . . ?
C23 N5 C21 118.2(5) . . ?
C22 N5 C21 122.3(5) . . ?
O11 C23 N5 120.2(6) . . ?
_database_code_depnum_ccdc_archive 'CCDC 971389'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Zr[(PDC)2(CH3OH)2](CH3OH)
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C17 H18 N2 O11 Zr'
_chemical_formula_weight         517.55

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_cell_length_a                   9.6801(2)
_cell_length_b                   18.9975(3)
_cell_length_c                   21.3644(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3928.87(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    173.0(2)

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2096
_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.014
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
; 
 SADABS(Blessing, 1995) 
;
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.99

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'Bruker SMART BREEZE'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      173.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_number            32977
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             4894
_reflns_number_gt                3357
_reflns_threshold_expression     >2sĬ)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0328P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4894
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.057
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0664
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_restrained_S_all      0.913
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.079

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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
Zr1 Zr 0.37039(2) 0.175975(12) 0.376314(10) 0.01589(7) Uani 1 1 d . . .
O1 O 0.19909(16) 0.22888(9) 0.41936(7) 0.0210(4) Uani 1 1 d . . .
O2 O 0.06795(19) 0.32480(10) 0.43225(9) 0.0346(5) Uani 1 1 d . . .
O3 O 0.47372(17) 0.17984(9) 0.28697(7) 0.0237(4) Uani 1 1 d . . .
O4 O 0.48417(17) 0.21263(10) 0.18678(8) 0.0267(4) Uani 1 1 d . . .
O5 O 0.46767(17) 0.27044(9) 0.41203(8) 0.0246(4) Uani 1 1 d . . .
O6 O 0.64492(18) 0.33230(9) 0.44789(9) 0.0301(4) Uani 1 1 d . . .
O7 O 0.42839(16) 0.06733(9) 0.36318(8) 0.0221(4) Uani 1 1 d . . .
O8 O 0.58962(17) -0.01594(9) 0.34958(8) 0.0280(4) Uani 1 1 d . . .
O9 O 0.19302(18) 0.12616(9) 0.32846(8) 0.0238(4) Uani 1 1 d . . .
O10 O 0.33044(19) 0.13039(10) 0.46888(9) 0.0239(4) Uani 1 1 d . . .
O11 O 0.9990(3) 0.05441(15) 0.61442(15) 0.0771(9) Uani 1 1 d . . .
H111 H 1.0429 0.0856 0.5969 0.116 Uiso 1 1 calc R . .
N1 N 0.28917(19) 0.26688(10) 0.31425(9) 0.0180(4) Uani 1 1 d . . .
N2 N 0.59771(19) 0.15702(10) 0.40446(9) 0.0187(4) Uani 1 1 d . . .
C1 C 0.1976(2) 0.31180(13) 0.33800(11) 0.0208(5) Uani 1 1 d . . .
C2 C 0.1527(3) 0.36994(14) 0.30434(12) 0.0266(6) Uani 1 1 d . . .
H2 H 0.091 0.402 0.3218 0.032 Uiso 1 1 calc R . .
C3 C 0.2023(3) 0.37890(15) 0.24398(13) 0.0316(6) Uani 1 1 d . . .
H3 H 0.1731 0.4171 0.2202 0.038 Uiso 1 1 calc R . .
C5 C 0.2961(3) 0.33071(14) 0.21887(12) 0.0273(6) Uani 1 1 d . . .
H5 H 0.3294 0.3357 0.1783 0.033 Uiso 1 1 calc R . .
C6 C 0.3379(2) 0.27555(13) 0.25616(11) 0.0202(5) Uani 1 1 d . . .
C7 C 0.1479(2) 0.28941(14) 0.40210(11) 0.0218(5) Uani 1 1 d . . .
C8 C 0.4397(2) 0.21920(13) 0.24037(11) 0.0215(5) Uani 1 1 d . . .
C9 C 0.6745(2) 0.20983(13) 0.42627(11) 0.0197(5) Uani 1 1 d . . .
C10 C 0.8131(2) 0.20115(14) 0.44007(11) 0.0246(6) Uani 1 1 d . . .
H10 H 0.8653 0.2382 0.4559 0.03 Uiso 1 1 calc R . .
C11 C 0.8714(3) 0.13610(15) 0.42965(12) 0.0283(6) Uani 1 1 d . . .
H11 H 0.9643 0.1288 0.4385 0.034 Uiso 1 1 calc R . .
C12 C 0.7923(2) 0.08174(14) 0.40608(12) 0.0257(6) Uani 1 1 d . . .
H12 H 0.8312 0.0378 0.3987 0.031 Uiso 1 1 calc R . .
C13 C 0.6547(2) 0.09396(13) 0.39375(11) 0.0197(5) Uani 1 1 d . . .
C14 C 0.5936(2) 0.27663(14) 0.43057(11) 0.0230(5) Uani 1 1 d . . .
C15 C 0.5528(2) 0.04240(13) 0.36606(11) 0.0201(5) Uani 1 1 d . . .
C16 C 0.1878(3) 0.07204(15) 0.28118(14) 0.0393(7) Uani 1 1 d . . .
H16A H 0.2127 0.0917 0.2414 0.059 Uiso 1 1 calc R . .
H16B H 0.0958 0.0532 0.2789 0.059 Uiso 1 1 calc R . .
H16C H 0.2512 0.0351 0.2918 0.059 Uiso 1 1 calc R . .
C17 C 0.3807(3) 0.06972(14) 0.50203(12) 0.0284(6) Uani 1 1 d . . .
H17A H 0.3626 0.0281 0.4779 0.043 Uiso 1 1 calc R . .
H17B H 0.3347 0.0662 0.5417 0.043 Uiso 1 1 calc R . .
H17C H 0.4784 0.0743 0.5086 0.043 Uiso 1 1 calc R . .
C18 C 0.8838(4) 0.0379(2) 0.57924(17) 0.0591(10) Uani 1 1 d . . .
H18A H 0.8338 0.0005 0.5992 0.089 Uiso 1 1 calc R . .
H18B H 0.912 0.0232 0.5382 0.089 Uiso 1 1 calc R . .
H18C H 0.8254 0.0786 0.5758 0.089 Uiso 1 1 calc R . .
H20 H 0.286(3) 0.1474(15) 0.4875(13) 0.025(9) Uiso 1 1 d . . .
H21 H 0.115(3) 0.1532(16) 0.3240(14) 0.042(9) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Zr1 O1 2.1460(16) . ?
Zr1 O3 2.1563(16) . ?
Zr1 O7 2.1573(17) . ?
Zr1 O5 2.1654(17) . ?
Zr1 O10 2.1933(18) . ?
Zr1 O9 2.2111(17) . ?
Zr1 N2 2.3094(19) . ?
Zr1 N1 2.315(2) . ?
O1 C7 1.305(3) . ?
O2 C7 1.211(3) . ?
O3 C8 1.288(3) . ?
O4 C8 1.229(3) . ?
O5 C14 1.288(3) . ?
O6 C14 1.226(3) . ?
O7 C15 1.296(3) . ?
O8 C15 1.216(3) . ?
O9 C16 1.442(3) . ?
O10 C17 1.438(3) . ?
O11 C18 1.381(4) . ?
N1 C1 1.331(3) . ?
N1 C6 1.338(3) . ?
N2 C9 1.333(3) . ?
N2 C13 1.339(3) . ?
C1 C2 1.388(3) . ?
C1 C7 1.512(3) . ?
C2 C3 1.387(4) . ?
C3 C5 1.397(4) . ?
C5 C6 1.377(3) . ?
C6 C8 1.494(3) . ?
C9 C10 1.383(3) . ?
C9 C14 1.494(3) . ?
C10 C11 1.377(4) . ?
C11 C12 1.381(4) . ?
C12 C13 1.377(3) . ?
C13 C15 1.511(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O3 136.21(6) . . ?
O1 Zr1 O7 134.82(6) . . ?
O3 Zr1 O7 78.27(6) . . ?
O1 Zr1 O5 78.28(6) . . ?
O3 Zr1 O5 94.70(7) . . ?
O7 Zr1 O5 136.51(6) . . ?
O1 Zr1 O10 70.26(7) . . ?
O3 Zr1 O10 153.31(7) . . ?
O7 Zr1 O10 77.61(7) . . ?
O5 Zr1 O10 94.95(7) . . ?
O1 Zr1 O9 78.38(6) . . ?
O3 Zr1 O9 88.02(7) . . ?
O7 Zr1 O9 74.48(6) . . ?
O5 Zr1 O9 148.79(6) . . ?
O10 Zr1 O9 96.37(7) . . ?
O1 Zr1 N2 134.24(6) . . ?
O3 Zr1 N2 78.10(6) . . ?
O7 Zr1 N2 68.70(7) . . ?
O5 Zr1 N2 67.86(7) . . ?
O10 Zr1 N2 82.62(7) . . ?
O9 Zr1 N2 142.52(7) . . ?
O1 Zr1 N1 68.51(6) . . ?
O3 Zr1 N1 67.98(6) . . ?
O7 Zr1 N1 136.69(6) . . ?
O5 Zr1 N1 74.41(7) . . ?
O10 Zr1 N1 138.69(7) . . ?
O9 Zr1 N1 77.92(7) . . ?
N2 Zr1 N1 126.10(7) . . ?
C7 O1 Zr1 125.78(15) . . ?
C8 O3 Zr1 125.84(15) . . ?
C14 O5 Zr1 126.58(16) . . ?
C15 O7 Zr1 125.83(15) . . ?
C16 O9 Zr1 131.02(16) . . ?
C17 O10 Zr1 134.52(16) . . ?
C1 N1 C6 120.6(2) . . ?
C1 N1 Zr1 119.09(16) . . ?
C6 N1 Zr1 120.23(15) . . ?
C9 N2 C13 120.2(2) . . ?
C9 N2 Zr1 120.34(15) . . ?
C13 N2 Zr1 119.19(15) . . ?
N1 C1 C2 121.4(2) . . ?
N1 C1 C7 112.1(2) . . ?
C2 C1 C7 126.4(2) . . ?
C1 C2 C3 118.1(2) . . ?
C2 C3 C5 120.1(2) . . ?
C6 C5 C3 117.9(2) . . ?
N1 C6 C5 121.8(2) . . ?
N1 C6 C8 110.7(2) . . ?
C5 C6 C8 127.5(2) . . ?
O2 C7 O1 125.5(2) . . ?
O2 C7 C1 121.9(2) . . ?
O1 C7 C1 112.5(2) . . ?
O4 C8 O3 124.9(2) . . ?
O4 C8 C6 120.9(2) . . ?
O3 C8 C6 114.2(2) . . ?
N2 C9 C10 121.7(2) . . ?
N2 C9 C14 111.6(2) . . ?
C10 C9 C14 126.6(2) . . ?
C11 C10 C9 118.0(2) . . ?
C10 C11 C12 120.2(2) . . ?
C13 C12 C11 118.7(2) . . ?
N2 C13 C12 121.1(2) . . ?
N2 C13 C15 112.2(2) . . ?
C12 C13 C15 126.6(2) . . ?
O6 C14 O5 123.7(2) . . ?
O6 C14 C9 122.6(2) . . ?
O5 C14 C9 113.6(2) . . ?
O8 C15 O7 126.3(2) . . ?
O8 C15 C13 120.9(2) . . ?
O7 C15 C13 112.9(2) . . ?

#===END
_database_code_depnum_ccdc_archive 'CCDC 971390'
