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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/4/10/93/4109338.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_4109338
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_common            SIMOF-4a
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 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                   11.1918(16)
_cell_length_b                   11.1918(16)
_cell_length_c                   31.561(6)
_cell_measurement_reflns_used    5424
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      4.02
_cell_volume                     3953.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78480
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_av_sigmaI/netI    0.0890
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            26182
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         4.02
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       Block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.090(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0544P)²+0.0436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                4598
_reflns_number_total             5424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070671ysi20070130_071413.cif
_cod_data_source_block           simof1a
_cod_database_code               4109338
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+1/4'
'-y+1/2, x+1/2, z+3/4'
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 -0.19934(3) -0.19934(3) 0.0000 0.00909(11) Uani 1 2 d S
O1 O 0.09362(19) -0.28421(18) 0.17613(6) 0.0237(5) Uani 1 1 d .
O2 O 0.24233(17) -0.17939(16) 0.20618(6) 0.0164(4) Uani 1 1 d .
O3 O -0.14289(18) 0.06167(17) 0.04810(6) 0.0173(4) Uani 1 1 d .
O4 O -0.32710(16) -0.06992(17) 0.01604(5) 0.0140(4) Uani 1 1 d .
O5 O -0.08475(17) -0.12941(16) 0.04521(6) 0.0143(4) Uani 1 1 d .
O6 O 0.2892(2) 0.23950(18) 0.16936(7) 0.0278(5) Uani 1 1 d .
O7 O 0.1800(2) 0.32798(19) 0.11923(8) 0.0361(6) Uani 1 1 d .
C1 C 0.0464(2) -0.1015(2) 0.11942(8) 0.0135(5) Uani 1 1 d .
H1 H 0.0119 -0.1759 0.1147 0.016 Uiso 1 1 calc R
C2 C 0.0135(2) -0.0050(2) 0.09400(7) 0.0133(5) Uani 1 1 d .
C3 C 0.0646(3) 0.1068(2) 0.10104(9) 0.0169(6) Uani 1 1 d .
H3 H 0.0412 0.1723 0.0849 0.020 Uiso 1 1 calc R
C4 C 0.1516(3) 0.1199(2) 0.13271(8) 0.0168(6) Uani 1 1 d .
C5 C 0.1832(3) 0.0223(2) 0.15775(8) 0.0161(5) Uani 1 1 d .
H5 H 0.2407 0.0315 0.1788 0.019 Uiso 1 1 calc R
C6 C 0.1301(2) -0.0881(2) 0.15172(8) 0.0137(5) Uani 1 1 d .
C7 C -0.0777(2) -0.0249(2) 0.05977(8) 0.0134(5) Uani 1 1 d .
C8 C 0.2070(3) 0.2409(2) 0.13934(9) 0.0201(6) Uani 1 1 d .
C9 C 0.1580(2) -0.1929(2) 0.18004(8) 0.0151(5) Uani 1 1 d .
C1S C 0.0247(3) -0.4309(3) 0.08262(10) 0.0321(8) Uani 1 1 d .
H1S1 H 0.0122 -0.4139 0.1121 0.048 Uiso 1 1 calc R
H1S2 H 0.0291 -0.5158 0.0786 0.048 Uiso 1 1 calc R
H1S3 H -0.0406 -0.3993 0.0664 0.048 Uiso 1 1 calc R
N2S N 0.1367(2) -0.3756(3) 0.06856(8) 0.0263(6) Uani 1 1 d .
C3S C 0.1452(3) -0.2760(3) 0.04582(9) 0.0233(7) Uani 1 1 d .
H3S H 0.0811 -0.2326 0.0351 0.028 Uiso 1 1 calc R
N4S N 0.2598(3) -0.2483(3) 0.04086(8) 0.0281(6) Uani 1 1 d .
C5S C 0.2493(4) -0.4126(4) 0.07869(15) 0.0523(12) Uani 1 1 d .
H5S H 0.2694 -0.4796 0.0946 0.063 Uiso 1 1 calc R
C6S C 0.3247(3) -0.3346(4) 0.06147(14) 0.0567(13) Uani 1 1 d .
H6S H 0.4076 -0.3379 0.0631 0.068 Uiso 1 1 calc R
C7S C 0.3057(4) -0.1425(3) 0.01802(10) 0.0358(8) Uani 1 1 d .
C8S C 0.3408(3) -0.0430(3) 0.04807(11) 0.0334(8) Uani 1 1 d .
H8S1 H 0.4037 -0.0706 0.0668 0.040 Uiso 1 1 calc R
H8S2 H 0.2726 -0.0207 0.0653 0.040 Uiso 1 1 calc R
C9S C 0.3847(4) 0.0665(4) 0.02288(14) 0.0492(11) Uani 1 1 d .
H9S1 H 0.4491 0.0422 0.0042 0.059 Uiso 1 1 calc R
H9S2 H 0.3199 0.0963 0.0054 0.059 Uiso 1 1 calc R
C10S C 0.4289(7) 0.1667(5) 0.0517(2) 0.099(2) Uani 1 1 d .
H10A H 0.3761 0.1743 0.0755 0.149 Uiso 1 1 calc R
H10B H 0.4303 0.2405 0.0362 0.149 Uiso 1 1 calc R
H10C H 0.5079 0.1483 0.0615 0.149 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'
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'
Ni Ni 0.3393 1.1124 '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
O2 Ni1 O2 91.93(11) 8_444 3_445
O2 Ni1 O5 175.72(7) 8_444 .
O2 Ni1 O5 89.00(8) 3_445 .
O2 Ni1 O5 89.00(8) 8_444 6
O2 Ni1 O5 175.72(7) 3_445 6
O5 Ni1 O5 90.38(11) . 6
O2 Ni1 O4 86.06(7) 8_444 .
O2 Ni1 O4 94.44(7) 3_445 .
O5 Ni1 O4 89.70(7) . .
O5 Ni1 O4 89.79(7) 6 .
O2 Ni1 O4 94.44(7) 8_444 6
O2 Ni1 O4 86.06(7) 3_445 6
O5 Ni1 O4 89.79(7) . 6
O5 Ni1 O4 89.70(7) 6 6
O4 Ni1 O4 179.28(11) . 6
C9 O2 Ni1 126.96(18) . 3_545
C7 O5 Ni1 129.86(17) . .
C6 C1 C2 121.0(3) . .
C3 C2 C1 119.7(2) . .
C3 C2 C7 121.7(2) . .
C1 C2 C7 118.6(2) . .
C2 C3 C4 119.5(2) . .
C5 C4 C3 119.9(3) . .
C5 C4 C8 121.5(2) . .
C3 C4 C8 118.6(2) . .
C6 C5 C4 120.8(3) . .
C5 C6 C1 119.1(2) . .
C5 C6 C9 121.6(2) . .
C1 C6 C9 119.3(2) . .
O5 C7 O3 124.6(2) . .
O5 C7 C2 116.3(2) . .
O3 C7 C2 119.1(2) . .
O7 C8 O6 124.3(3) . .
O7 C8 C4 123.6(3) . .
O6 C8 C4 112.1(2) . .
O1 C9 O2 126.1(2) . .
O1 C9 C6 117.2(2) . .
O2 C9 C6 116.7(2) . .
C3S N2S C5S 108.4(3) . .
C3S N2S C1S 125.3(3) . .
C5S N2S C1S 126.2(3) . .
N4S C3S N2S 109.1(3) . .
C3S N4S C6S 106.9(3) . .
C3S N4S C7S 125.4(3) . .
C6S N4S C7S 127.6(3) . .
C6S C5S N2S 106.9(3) . .
C5S C6S N4S 108.6(3) . .
N4S C7S C8S 111.9(3) . .
C7S C8S C9S 110.1(3) . .
C10S C9S C8S 112.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.0448(18) 8_444
Ni1 O2 2.0448(18) 3_445
Ni1 O5 2.0722(18) .
Ni1 O5 2.0722(18) 6
Ni1 O4 2.0974(18) .
Ni1 O4 2.0974(18) 6
O1 C9 1.257(3) .
O2 C9 1.263(3) .
O2 Ni1 2.0448(18) 3_545
O3 C7 1.268(3) .
O5 C7 1.259(3) .
O6 C8 1.321(4) .
O7 C8 1.202(3) .
C1 C6 1.393(4) .
C1 C2 1.395(4) .
C2 C3 1.394(4) .
C2 C7 1.503(4) .
C3 C4 1.403(4) .
C4 C5 1.394(4) .
C4 C8 1.503(4) .
C5 C6 1.384(4) .
C6 C9 1.507(4) .
C1S N2S 1.467(4) .
N2S C3S 1.329(4) .
N2S C5S 1.364(4) .
C3S N4S 1.328(4) .
N4S C6S 1.372(4) .
N4S C7S 1.479(4) .
C5S C6S 1.330(6) .
C7S C8S 1.514(5) .
C8S C9S 1.541(5) .
C9S C10S 1.527(7) .
