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#$Date: 2016-03-21 19:11:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178839 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/93/4109337.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_4109337
loop_
_publ_author_name
'Zhuojia Lin'
'Alexandra M. Z. Slawin'
'Russell E. Morris'
_publ_contact_author_address
;University of St Andrews
EaStChem School of Chemistry
Purdie Building
St Andrews KY169ST
;
_publ_contact_author_email       rem1@st-and.ac.uk
_publ_contact_author_fax         01334463808
_publ_contact_author_name        'Russell Morris'
_publ_contact_author_phone       01334463818
_publ_section_title
;
 Chiral Induction in the Ionothermal Synthesis of a 3-D Coordination
 Polymer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4880
_journal_page_last               4881
_journal_paper_doi               10.1021/ja070671y
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C34 H42 N4 Ni O14'
_chemical_formula_weight         789.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1813(4)
_cell_length_b                   11.1813(4)
_cell_length_c                   31.5520(13)
_cell_measurement_reflns_used    3738
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.66
_cell_volume                     3944.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  Rigaku
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            22316
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       Block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0320P)²+1.6138P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                3599
_reflns_number_total             3738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070671ysi20070130_071356.cif
_cod_data_source_block           SIMOF-1
_cod_database_code               4109337
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+3/4'
'-y+1/2, x+1/2, z+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
Ni1 Ni 1.300509(18) 0.699491(18) 0.7500 0.00914(8) Uani 1 2 d S
C1 C 1.08804(15) 0.86952(15) 0.65144(5) 0.0133(4) Uani 1 1 d .
C2 C 1.10120(15) 0.95329(16) 0.61925(5) 0.0130(4) Uani 1 1 d .
H2 H 1.1756 0.9880 0.6146 0.016 Uiso 1 1 calc R
C3 C 1.00444(15) 0.98601(15) 0.59386(5) 0.0127(3) Uani 1 1 d .
C4 C 0.89318(15) 0.93447(16) 0.60082(5) 0.0146(4) Uani 1 1 d .
H4 H 0.8278 0.9575 0.5846 0.017 Uiso 1 1 calc R
C5 C 0.87993(16) 0.84763(16) 0.63244(5) 0.0157(4) Uani 1 1 d .
C6 C 0.97692(15) 0.81608(16) 0.65762(5) 0.0140(4) Uani 1 1 d .
H6 H 0.9675 0.7589 0.6788 0.017 Uiso 1 1 calc R
C7 C 1.19298(16) 0.84175(15) 0.68010(5) 0.0136(4) Uani 1 1 d .
C8 C 1.02493(15) 1.07796(15) 0.55959(5) 0.0120(4) Uani 1 1 d .
C9 C 0.75935(15) 0.79186(17) 0.63906(5) 0.0176(4) Uani 1 1 d .
O1 O 1.17961(10) 0.75733(11) 0.70607(4) 0.0150(3) Uani 1 1 d .
O1W O 1.42976(12) 0.82716(11) 0.73439(4) 0.0129(3) Uani 1 1 d .
H1WB H 1.388(2) 0.860(2) 0.7137(8) 0.037(7) Uiso 1 1 d .
H1WA H 1.479(3) 0.785(3) 0.7219(8) 0.045(8) Uiso 1 1 d .
O2 O 1.28413(11) 0.90650(12) 0.67608(4) 0.0206(3) Uani 1 1 d .
O3 O 1.12936(10) 1.08488(11) 0.54518(4) 0.0136(3) Uani 1 1 d .
O4 O 0.93786(11) 1.14247(12) 0.54787(4) 0.0157(3) Uani 1 1 d .
O5 O 0.67146(11) 0.81857(14) 0.61893(4) 0.0285(3) Uani 1 1 d .
O6 O 0.76090(12) 0.71043(13) 0.66939(4) 0.0241(3) Uani 1 1 d .
H1 H 0.686(3) 0.683(3) 0.6765(9) 0.058(8) Uiso 1 1 d .
N1 N 1.37503(15) 0.86306(15) 0.56852(5) 0.0215(4) Uani 1 1 d .
N2 N 1.24794(16) 0.74042(15) 0.54078(5) 0.0240(4) Uani 1 1 d .
C1S C 1.43032(19) 0.97489(18) 0.58282(6) 0.0263(4) Uani 1 1 d .
H1SA H 1.3873 1.0416 0.5712 0.040 Uiso 1 1 calc R
H1SB H 1.5119 0.9777 0.5734 0.040 Uiso 1 1 calc R
H1SC H 1.4280 0.9787 0.6132 0.040 Uiso 1 1 calc R
C2S C 1.27600(17) 0.85456(17) 0.54563(6) 0.0195(4) Uani 1 1 d .
H2SA H 1.2330 0.9187 0.5347 0.023 Uiso 1 1 calc R
C3S C 1.4123(2) 0.7496(2) 0.57878(9) 0.0415(6) Uani 1 1 d .
H3SA H 1.4792 0.7295 0.5947 0.050 Uiso 1 1 calc R
C4S C 1.3335(2) 0.6735(2) 0.56141(8) 0.0454(7) Uani 1 1 d .
H4SA H 1.3363 0.5905 0.5630 0.054 Uiso 1 1 calc R
C5S C 1.14210(19) 0.6938(2) 0.51844(6) 0.0287(5) Uani 1 1 d .
H5SA H 1.1656 0.6251 0.5016 0.034 Uiso 1 1 calc R
H5SB H 1.1127 0.7547 0.4991 0.034 Uiso 1 1 calc R
C6S C 1.04235(19) 0.6577(2) 0.54792(6) 0.0273(5) Uani 1 1 d .
H6SA H 1.0197 0.7256 0.5653 0.033 Uiso 1 1 calc R
H6SB H 1.0702 0.5947 0.5666 0.033 Uiso 1 1 calc R
C7S C 0.9337(2) 0.6138(2) 0.52337(8) 0.0366(6) Uani 1 1 d .
H7SA H 0.9037 0.6788 0.5060 0.044 Uiso 1 1 calc R
H7SB H 0.9586 0.5500 0.5045 0.044 Uiso 1 1 calc R
C8S C 0.8339(3) 0.5685(4) 0.55100(11) 0.0756(11) Uani 1 1 d .
H8SA H 0.7688 0.5422 0.5335 0.113 Uiso 1 1 calc R
H8SB H 0.8071 0.6317 0.5693 0.113 Uiso 1 1 calc R
H8SC H 0.8622 0.5028 0.5678 0.113 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
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
O1 Ni1 O1 92.37(7) 5_776 .
O1 Ni1 O3 88.82(5) 5_776 8_745
O1 Ni1 O3 175.64(5) . 8_745
O1 Ni1 O3 175.64(5) 5_776 4_746
O1 Ni1 O3 88.82(5) . 4_746
O3 Ni1 O3 90.30(7) 8_745 4_746
O1 Ni1 O1W 94.67(5) 5_776 5_776
O1 Ni1 O1W 85.80(5) . 5_776
O3 Ni1 O1W 89.92(5) 8_745 5_776
O3 Ni1 O1W 89.60(5) 4_746 5_776
O1 Ni1 O1W 85.80(5) 5_776 .
O1 Ni1 O1W 94.67(5) . .
O3 Ni1 O1W 89.60(5) 8_745 .
O3 Ni1 O1W 89.92(5) 4_746 .
O1W Ni1 O1W 179.31(8) 5_776 .
C2 C1 C6 119.09(16) . .
C2 C1 C7 119.53(15) . .
C6 C1 C7 121.34(15) . .
C1 C2 C3 120.96(16) . .
C1 C2 H2 119.5 . .
C3 C2 H2 119.5 . .
C4 C3 C2 119.68(16) . .
C4 C3 C8 122.14(15) . .
C2 C3 C8 118.18(15) . .
C3 C4 C5 119.69(16) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
C6 C5 C4 120.05(16) . .
C6 C5 C9 121.08(16) . .
C4 C5 C9 118.86(16) . .
C5 C6 C1 120.49(16) . .
C5 C6 H6 119.8 . .
C1 C6 H6 119.8 . .
O2 C7 O1 126.44(16) . .
O2 C7 C1 116.77(14) . .
O1 C7 C1 116.78(15) . .
O3 C8 O4 125.03(16) . .
O3 C8 C3 116.27(15) . .
O4 C8 C3 118.70(15) . .
O5 C9 O6 124.20(17) . .
O5 C9 C5 123.74(16) . .
O6 C9 C5 112.06(15) . .
C7 O1 Ni1 126.94(11) . .
Ni1 O1W H1WB 95.4(17) . .
Ni1 O1W H1WA 101(2) . .
H1WB O1W H1WA 104(2) . .
C8 O3 Ni1 129.76(11) . 4_756
C9 O6 H1 113.0(18) . .
C2S N1 C3S 108.38(18) . .
C2S N1 C1S 125.53(17) . .
C3S N1 C1S 125.97(17) . .
C2S N2 C4S 107.72(18) . .
C2S N2 C5S 125.95(17) . .
C4S N2 C5S 126.30(19) . .
N1 C1S H1SA 109.5 . .
N1 C1S H1SB 109.5 . .
H1SA C1S H1SB 109.5 . .
N1 C1S H1SC 109.5 . .
H1SA C1S H1SC 109.5 . .
H1SB C1S H1SC 109.5 . .
N2 C2S N1 109.29(17) . .
N2 C2S H2SA 125.4 . .
N1 C2S H2SA 125.4 . .
C4S C3S N1 106.92(19) . .
C4S C3S H3SA 126.5 . .
N1 C3S H3SA 126.5 . .
C3S C4S N2 107.7(2) . .
C3S C4S H4SA 126.2 . .
N2 C4S H4SA 126.2 . .
N2 C5S C6S 113.20(16) . .
N2 C5S H5SA 108.9 . .
C6S C5S H5SA 108.9 . .
N2 C5S H5SB 108.9 . .
C6S C5S H5SB 108.9 . .
H5SA C5S H5SB 107.8 . .
C5S C6S C7S 111.27(17) . .
C5S C6S H6SA 109.4 . .
C7S C6S H6SA 109.4 . .
C5S C6S H6SB 109.4 . .
C7S C6S H6SB 109.4 . .
H6SA C6S H6SB 108.0 . .
C8S C7S C6S 113.9(2) . .
C8S C7S H7SA 108.8 . .
C6S C7S H7SA 108.8 . .
C8S C7S H7SB 108.8 . .
C6S C7S H7SB 108.8 . .
H7SA C7S H7SB 107.7 . .
C7S C8S H8SA 109.5 . .
C7S C8S H8SB 109.5 . .
H8SA C8S H8SB 109.5 . .
C7S C8S H8SC 109.5 . .
H8SA C8S H8SC 109.5 . .
H8SB C8S H8SC 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.0413(12) 5_776
Ni1 O1 2.0413(12) .
Ni1 O3 2.0711(12) 8_745
Ni1 O3 2.0711(12) 4_746
Ni1 O1W 2.0902(12) 5_776
Ni1 O1W 2.0902(12) .
C1 C2 1.389(2) .
C1 C6 1.392(2) .
C1 C7 1.513(2) .
C2 C3 1.395(2) .
C2 H2 0.9300 .
C3 C4 1.389(2) .
C3 C8 1.510(2) .
C4 C5 1.400(3) .
C4 H4 0.9300 .
C5 C6 1.390(2) .
C5 C9 1.500(2) .
C6 H6 0.9300 .
C7 O2 1.257(2) .
C7 O1 1.259(2) .
C8 O3 1.255(2) .
C8 O4 1.267(2) .
C9 O5 1.208(2) .
C9 O6 1.321(2) .
O1W H1WB 0.88(3) .
O1W H1WA 0.82(3) .
O3 Ni1 2.0711(12) 4_756
O6 H1 0.92(3) .
N1 C2S 1.325(3) .
N1 C3S 1.374(3) .
N1 C1S 1.466(3) .
N2 C2S 1.323(3) .
N2 C4S 1.378(3) .
N2 C5S 1.473(3) .
C1S H1SA 0.9600 .
C1S H1SB 0.9600 .
C1S H1SC 0.9600 .
C2S H2SA 0.9300 .
C3S C4S 1.342(4) .
C3S H3SA 0.9300 .
C4S H4SA 0.9300 .
C5S C6S 1.508(3) .
C5S H5SA 0.9700 .
C5S H5SB 0.9700 .
C6S C7S 1.522(3) .
C6S H6SA 0.9700 .
C6S H6SB 0.9700 .
C7S C8S 1.504(4) .
C7S H7SA 0.9700 .
C7S H7SB 0.9700 .
C8S H8SA 0.9600 .
C8S H8SB 0.9600 .
C8S H8SC 0.9600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WB O2 0.88(3) 1.74(3) 2.6121(18) 169(2) .
O1W H1WA O4 0.82(3) 1.95(3) 2.7370(18) 160(3) 4_746
O6 H1 O4 0.92(3) 1.67(3) 2.5659(17) 165(3) 4_646
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O1 C7 C1 C2 -173.50(15)
O3 C8 C3 C4 -153.70(16)
O5 C9 C5 C6 177.74(18)
