#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/82/7018262.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_7018262
loop_
_publ_author_name
'Zheng, Wenxu'
'Wei, Yongqin'
'Xiao, Xueying'
'Wu, Kechen'
_publ_section_title
;
 Spontaneous asymmetric crystallization of a quartz-type framework from
 achiral precursors.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3138
_journal_page_last               3140
_journal_paper_doi               10.1039/c2dt12238c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C4 H12 N3 Ni1.5 O10'
_chemical_formula_weight         350.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.92450(10)
_cell_length_b                   11.92450(10)
_cell_length_c                   16.3020(5)
_cell_measurement_reflns_used    5263
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1836
_cell_volume                     2007.48(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Saturn70
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15752
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8247
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.986
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0860P)²+1.1088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                2908
_reflns_number_total             3077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12238c.txt
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P3(1)21
_cod_original_formula_sum        'C4 H12 N3 Ni1.50 O10'
_cod_database_code               7018262
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
'y, x, -z'
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 0.62675(6) 0.62675(6) 0.0000 0.01644(18) Uani 1 2 d S
Ni2 Ni 0.45662(6) 0.50488(5) 0.19226(3) 0.02117(16) Uani 1 1 d .
N3 N 0.5745(3) 0.7195(3) 0.07986(19) 0.0182(7) Uani 1 1 d .
O1 O 0.4568(3) 0.9319(3) 0.24863(17) 0.0231(6) Uani 1 1 d .
O3 O 0.6984(4) 0.8094(3) -0.05657(18) 0.0295(8) Uani 1 1 d .
O2 O 0.4303(4) 0.7532(3) 0.3110(2) 0.0371(9) Uani 1 1 d .
N1 N 0.5723(4) 0.8952(4) 0.1183(2) 0.0240(8) Uani 1 1 d .
O3W O 0.2872(4) 0.4355(4) 0.1248(2) 0.0410(9) Uani 1 1 d .
O1W O 0.6270(4) 0.5757(4) 0.2587(3) 0.0485(10) Uani 1 1 d .
N2 N 0.5127(4) 0.6909(3) 0.1537(2) 0.0190(7) Uani 1 1 d .
C2 C 0.5139(4) 0.8003(4) 0.1750(2) 0.0201(8) Uani 1 1 d .
C3 C 0.6065(4) 0.8388(4) 0.0610(2) 0.0211(8) Uani 1 1 d .
C1 C 0.4616(5) 0.8265(4) 0.2519(3) 0.0219(9) Uani 1 1 d .
O2W O 0.3504(5) 0.5033(4) 0.2894(2) 0.0488(12) Uani 1 1 d .
O4 O 0.7192(6) 1.0045(4) -0.0388(3) 0.0611(16) Uani 1 1 d .
C4 C 0.6801(6) 0.8908(5) -0.0172(3) 0.0312(11) Uani 1 1 d .
O4W O 0.8416(5) 0.8002(6) 0.2089(3) 0.0604(13) Uani 1 1 d .
O5W O 0.6347(11) 0.5464(13) 0.4276(5) 0.152(5) Uani 1 1 d .
O6W O 0.1371(14) 0.1732(9) 0.0979(7) 0.225(7) Uani 1 1 d .
H5WB H 0.6865 0.6278 0.4271 0.269 Uiso 1 1 d R
H2WA H 0.3039 0.4562 0.3288 0.269 Uiso 1 1 d R
H2WB H 0.4268 0.5313 0.3074 0.269 Uiso 1 1 d R
H6WB H 0.1464 0.1964 0.1479 0.269 Uiso 1 1 d R
H3WB H 0.3008 0.4888 0.0863 0.269 Uiso 1 1 d R
H1WA H 0.6001 0.5950 0.3019 0.269 Uiso 1 1 d R
H4WB H 0.8977 0.7861 0.2313 0.269 Uiso 1 1 d R
H6WA H 0.0578 0.1414 0.0854 0.269 Uiso 1 1 d R
H3WA H 0.2468 0.3623 0.1015 0.269 Uiso 1 1 d R
H4WA H 0.8125 0.7462 0.1698 0.269 Uiso 1 1 d R
H5WA H 0.6344 0.5057 0.4710 0.269 Uiso 1 1 d R
H1WB H 0.6897 0.6498 0.2457 0.269 Uiso 1 1 d 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
N3 Ni1 N3 166.1(2) . 6
N3 Ni1 O1 105.02(13) . 3_564
N3 Ni1 O1 84.42(12) 6 3_564
N3 Ni1 O1 84.42(12) . 5_655
N3 Ni1 O1 105.02(13) 6 5_655
O1 Ni1 O1 95.73(18) 3_564 5_655
N3 Ni1 O3 92.02(13) . 6
N3 Ni1 O3 77.97(13) 6 6
O1 Ni1 O3 162.29(11) 3_564 6
O1 Ni1 O3 90.60(13) 5_655 6
N3 Ni1 O3 77.97(12) . .
N3 Ni1 O3 92.02(13) 6 .
O1 Ni1 O3 90.60(13) 3_564 .
O1 Ni1 O3 162.29(11) 5_655 .
O3 Ni1 O3 88.3(2) 6 .
O2W Ni2 N1 94.30(15) . 5_655
O2W Ni2 N2 96.49(14) . .
N1 Ni2 N2 168.97(15) 5_655 .
O2W Ni2 O1W 94.38(19) . .
N1 Ni2 O1W 87.06(16) 5_655 .
N2 Ni2 O1W 89.81(16) . .
O2W Ni2 O3W 86.04(19) . .
N1 Ni2 O3W 93.35(17) 5_655 .
N2 Ni2 O3W 89.71(15) . .
O1W Ni2 O3W 179.39(18) . .
O2W Ni2 O1 170.52(16) . 5_655
N1 Ni2 O1 79.26(13) 5_655 5_655
N2 Ni2 O1 90.30(12) . 5_655
O1W Ni2 O1 92.25(16) . 5_655
O3W Ni2 O1 87.39(14) . 5_655
O2W Ni2 H2WB 24.6 . .
N1 Ni2 H2WB 92.8 5_655 .
N2 Ni2 H2WB 96.0 . .
O1W Ni2 H2WB 69.8 . .
O3W Ni2 H2WB 110.6 . .
O1 Ni2 H2WB 160.9 5_655 .
C3 N3 N2 107.8(3) . .
C3 N3 Ni1 116.4(3) . .
N2 N3 Ni1 135.8(3) . .
C1 O1 Ni1 127.9(3) . 2_665
C1 O1 Ni2 115.0(3) . 5_665
Ni1 O1 Ni2 117.12(13) 2_665 5_665
C4 O3 Ni1 115.6(3) . .
C3 N1 C2 102.5(3) . .
C3 N1 Ni2 143.8(3) . 5_665
C2 N1 Ni2 112.0(3) . 5_665
Ni2 O3W H3WB 108.1 . .
Ni2 O3W H3WA 126.0 . .
H3WB O3W H3WA 103.7 . .
Ni2 O1W H1WA 96.7 . .
Ni2 O1W H1WB 117.7 . .
H1WA O1W H1WB 100.3 . .
C2 N2 N3 104.1(3) . .
C2 N2 Ni2 143.6(3) . .
N3 N2 Ni2 112.4(2) . .
N2 C2 N1 112.8(4) . .
N2 C2 C1 127.9(4) . .
N1 C2 C1 119.3(4) . .
N3 C3 N1 112.8(4) . .
N3 C3 C4 116.2(4) . .
N1 C3 C4 130.9(4) . .
O2 C1 O1 125.6(4) . .
O2 C1 C2 121.2(4) . .
O1 C1 C2 113.2(4) . .
Ni2 O2W H2WA 142.8 . .
Ni2 O2W H2WB 73.9 . .
H2WA O2W H2WB 102.5 . .
O4 C4 O3 125.2(4) . .
O4 C4 C3 121.1(4) . .
O3 C4 C3 113.8(4) . .
H4WB O4W H4WA 103.7 . .
H5WB O5W H5WA 116.8 . .
H6WB O6W H6WA 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N3 1.999(3) .
Ni1 N3 1.999(3) 6
Ni1 O1 2.090(3) 3_564
Ni1 O1 2.090(3) 5_655
Ni1 O3 2.112(3) 6
Ni1 O3 2.112(3) .
Ni2 O2W 2.022(3) .
Ni2 N1 2.054(4) 5_655
Ni2 N2 2.068(3) .
Ni2 O1W 2.073(4) .
Ni2 O3W 2.075(4) .
Ni2 O1 2.153(3) 5_655
Ni2 H2WB 1.9642 .
N3 C3 1.313(6) .
N3 N2 1.364(4) .
O1 C1 1.287(5) .
O1 Ni1 2.090(3) 2_665
O1 Ni2 2.153(3) 5_665
O3 C4 1.271(6) .
O2 C1 1.227(5) .
N1 C3 1.329(5) .
N1 C2 1.353(5) .
N1 Ni2 2.054(4) 5_665
O3W H3WB 0.8493 .
O3W H3WA 0.8471 .
O1W H1WA 0.8518 .
O1W H1WB 0.8509 .
N2 C2 1.343(5) .
C2 C1 1.502(5) .
C3 C4 1.495(6) .
O2W H2WA 0.8509 .
O2W H2WB 0.8501 .
O4 C4 1.244(6) .
O4W H4WB 0.8493 .
O4W H4WA 0.8478 .
O5W H5WB 0.8509 .
O5W H5WA 0.8572 .
O6W H6WB 0.8498 .
O6W H6WA 0.8500 .
