#------------------------------------------------------------------------------
#$Date: 2016-03-21 00:21:50 +0100 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/00/17/4001756.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_4001756
loop_
_publ_author_name
'Jeong, Seok'
'Kim, Dongwook'
'Song, Xiaokai'
'Choi, Min'
'Park, Noejung'
'Lah, Myoung Soo'
_publ_section_title
;
 Postsynthetic Exchanges of the Pillaring Ligand in Three-Dimensional
 Metal--Organic Frameworks
;
_journal_issue                   7
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1047
_journal_paper_doi               10.1021/cm303624p
_journal_volume                  25
_journal_year                    2013
_chemical_formula_sum            'C15 H16 N2 Ni O6'
_chemical_formula_weight         379.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           189
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6 -2'
_symmetry_space_group_name_H-M   'P -6 2 m'
_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            3
_cell_length_a                   16.666(2)
_cell_length_b                   16.666(2)
_cell_length_c                   7.0012(14)
_cell_measurement_reflns_used    1418
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      52.78
_cell_measurement_theta_min      7.47
_cell_volume                     1684.1(4)
_computing_cell_refinement       'Rigaku Rapid Auto'
_computing_data_collection       'Rigaku Rapid Auto'
_computing_data_reduction        'Rigaku Rapid Auto'
_computing_molecular_graphics    'Diamond 3.2h,ORTEP3'
_computing_publication_material  WinGX
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'imaging plate'
_diffrn_measurement_method       'omega 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  0.1531
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16600
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.9569
_exptl_absorpt_correction_T_min  0.8285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rigaku Rapid Auto'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.914
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0866
_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/[\s^2^(Fo^2^)+(0.1666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2362
_reflns_number_gt                1261
_reflns_number_total             1476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm303624p_si_002.cif
_cod_data_source_block           l12_025
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1684.1(5)
_cod_original_sg_symbol_H-M      P-62m
_cod_database_code               4001756
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'y, x, z'
'-x, -x+y, z'
'x-y, -y, z'
'x, y, -z'
'-x+y, -x, -z'
'-y, x-y, -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 0.67827(7) 1.0000 0.5000 0.0312(4) Uani 1 4 d S
O1 O 0.8274(4) 1.0777(4) 0.5000 0.0412(14) Uani 1 2 d S
O2 O 0.5510(4) 0.8853(4) 0.5000 0.0410(16) Uani 1 2 d S
O3 O 0.4363(5) 0.9185(5) 0.5000 0.0561(18) Uani 1 2 d S
C1 C 0.8253(8) 1.0000 0.5000 0.032(2) Uani 1 4 d S
C2 C 0.9161(7) 1.0000 0.5000 0.034(2) Uani 1 4 d S
C3 C 1.0000 1.0828(6) 0.5000 0.033(2) Uani 1 4 d S
H3 H 1.0000 1.1398 0.5000 0.039 Uiso 1 4 calc SR
C4 C 0.4664(7) 0.8614(5) 0.5000 0.045(2) Uani 1 2 d S
C5 C 0.3984(6) 0.7612(6) 0.5000 0.0405(19) Uani 1 2 d S
C6 C 0.4270(6) 0.6962(6) 0.5000 0.0393(19) Uani 1 2 d S
H6 H 0.4914 0.7164 0.5000 0.047 Uiso 1 2 calc SR
N1 N 0.6760(3) 1.0000 0.1857(9) 0.0311(12) Uani 1 2 d S
C11 C 0.7546(6) 1.0815(5) 0.1076(11) 0.062(2) Uani 1 1 d .
H11A H 0.8123 1.0848 0.1540 0.075 Uiso 1 1 calc R
H11B H 0.7540 1.1372 0.1540 0.075 Uiso 1 1 calc R
C12 C 0.5934(5) 1.0000 0.1080(13) 0.062(3) Uani 1 2 d S
H12A H 0.5923 1.0555 0.1548 0.075 Uiso 0.50 1 calc PR
H12B H 0.5368 0.9445 0.1548 0.075 Uiso 0.50 1 calc PR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0279(5) 0.0253(7) 0.0394(7) 0.000 0.000 0.0127(3)
O1 0.032(3) 0.040(4) 0.060(3) 0.000 0.000 0.024(3)
O2 0.026(3) 0.037(3) 0.065(4) 0.000 0.000 0.019(3)
O3 0.042(4) 0.033(3) 0.102(5) 0.000 0.000 0.026(3)
C1 0.041(4) 0.031(6) 0.020(4) 0.000 0.000 0.016(3)
C2 0.037(4) 0.043(6) 0.024(4) 0.000 0.000 0.021(3)
C3 0.053(7) 0.032(4) 0.021(4) 0.000 0.000 0.026(3)
C4 0.043(6) 0.028(4) 0.060(5) 0.000 0.000 0.014(4)
C5 0.032(4) 0.033(4) 0.051(5) 0.000 0.000 0.012(3)
C6 0.030(4) 0.034(4) 0.060(5) 0.000 0.000 0.020(3)
N1 0.0255(18) 0.024(3) 0.043(3) 0.000 -0.0007(17) 0.0122(13)
C11 0.061(4) 0.051(4) 0.037(4) -0.002(3) 0.001(3) 0.000(3)
C12 0.057(4) 0.118(10) 0.033(4) 0.000 -0.001(3) 0.059(5)
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 109.7(3) . 4_676
O2 Ni1 O1 156.5(2) . .
O2 Ni1 O1 93.8(2) 4_676 .
O2 Ni1 O1 93.8(2) . 4_676
O2 Ni1 O1 156.5(2) 4_676 4_676
O1 Ni1 O1 62.8(3) . 4_676
O2 Ni1 N1 89.44(7) . .
O2 Ni1 N1 89.44(7) 4_676 .
O1 Ni1 N1 90.84(11) . .
O1 Ni1 N1 90.84(11) 4_676 .
O2 Ni1 N1 89.44(7) . 4_676
O2 Ni1 N1 89.44(7) 4_676 4_676
O1 Ni1 N1 90.84(11) . 4_676
O1 Ni1 N1 90.83(11) 4_676 4_676
N1 Ni1 N1 178.0(3) . 4_676
O2 Ni1 C1 125.14(15) . .
O2 Ni1 C1 125.14(15) 4_676 .
O1 Ni1 C1 31.39(16) . .
O1 Ni1 C1 31.38(16) 4_676 .
N1 Ni1 C1 90.98(13) . .
N1 Ni1 C1 90.98(13) 4_676 .
C1 O1 Ni1 87.2(6) . .
C4 O2 Ni1 141.0(5) . .
O1 C1 O1 122.7(11) 4_676 .
O1 C1 C2 118.6(6) 4_676 .
O1 C1 C2 118.6(6) . .
O1 C1 Ni1 61.4(6) 4_676 .
O1 C1 Ni1 61.4(6) . .
C2 C1 Ni1 180.000(1) . .
C3 C2 C3 118.7(12) 2_765 .
C3 C2 C1 120.6(6) 2_765 .
C3 C2 C1 120.6(6) . .
C2 C3 C2 121.3(12) . 3_675
O2 C4 O3 124.0(8) . .
O2 C4 C5 117.5(8) . .
O3 C4 C5 118.5(9) . .
C6 C5 C6 119.1(8) . 2_665
C6 C5 C4 121.0(9) . .
C6 C5 C4 119.9(9) 2_665 .
C5 C6 C5 120.9(8) . 3_565
C11 N1 C11 109.2(8) . 9_675
C11 N1 C12 105.6(5) . .
C11 N1 C12 105.6(5) 9_675 .
C11 N1 Ni1 111.8(4) . .
C11 N1 Ni1 111.8(4) 9_675 .
C12 N1 Ni1 112.5(5) . .
N1 C11 C11 112.3(4) . 10
N1 C12 C12 111.5(4) . 4_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O2 2.025(7) .
Ni1 O2 2.025(7) 4_676
Ni1 O1 2.153(5) .
Ni1 O1 2.153(5) 4_676
Ni1 N1 2.201(7) .
Ni1 N1 2.201(7) 4_676
Ni1 C1 2.450(13) .
O1 C1 1.277(8) .
O2 C4 1.258(11) .
O3 C4 1.278(11) .
C1 O1 1.277(8) 4_676
C1 C2 1.514(16) .
C2 C3 1.389(7) 2_765
C2 C3 1.389(7) .
C3 C2 1.389(7) 3_675
C4 C5 1.478(12) .
C5 C6 1.383(13) .
C5 C6 1.395(12) 2_665
C6 C5 1.395(12) 3_565
N1 C11 1.442(8) .
N1 C11 1.442(8) 9_675
N1 C12 1.480(10) .
C11 C11 1.507(16) 10
C12 C12 1.513(18) 4_675
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.016 0.618 -0.355 743.6 18.1
