#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:48:51 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180277 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/63/7116320.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_7116320
loop_
_publ_author_name
'Xiao-Meng Zhang'
'Chao-Wei Zhao'
'Jian-Ping Ma'
'Yang Yu'
'Qi-Kui Liu'
'Yu-Bin Dong'
_publ_section_title
;
 A Ni(II)-MOF: reversible guest adsorption and heterogeneous catalytic
 properties for silylcyanation of aromatic aldehydes
;
_journal_name_full               Chem.Commun.
_journal_page_first              839
_journal_paper_doi               10.1039/C4cc08003C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C38 H32 Cl2 N12 Ni'
_chemical_formula_weight         786.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 130.367(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.101(14)
_cell_length_b                   20.893(16)
_cell_length_c                   13.626(11)
_cell_measurement_reflns_used    3345
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.096
_cell_measurement_theta_min      2.949
_cell_volume                     3926(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10339
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.8604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0432
_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)+(0.0705P)²+0.5911P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                2868
_reflns_number_total             3686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc08003c2.cif
_cod_data_source_block           130507bm
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7116320
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'
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
C1 C 0.0598(3) 0.14301(14) 1.0078(3) 0.0415(8) Uani 1 1 d .
H1 H 0.0406 0.1554 1.0539 0.050 Uiso 1 1 calc R
C2 C 0.0871(2) 0.08517(13) 0.9100(3) 0.0320(7) Uani 1 1 d .
H2 H 0.0926 0.0506 0.8721 0.038 Uiso 1 1 calc R
C3 C 0.1573(2) 0.17023(14) 0.8625(3) 0.0326(7) Uani 1 1 d .
C4 C 0.1283(2) 0.22977(14) 0.8036(3) 0.0350(7) Uani 1 1 d .
H4 H 0.0824 0.2538 0.7981 0.042 Uiso 1 1 calc R
C5 C 0.1695(2) 0.25229(14) 0.7535(3) 0.0337(7) Uani 1 1 d .
C6 C 0.2407(2) 0.21665(14) 0.7660(3) 0.0320(7) Uani 1 1 d .
C7 C 0.2699(2) 0.15789(15) 0.8273(3) 0.0381(7) Uani 1 1 d .
H7 H 0.3178 0.1345 0.8364 0.046 Uiso 1 1 calc R
C8 C 0.2271(2) 0.13428(15) 0.8749(3) 0.0379(7) Uani 1 1 d .
H8 H 0.2451 0.0945 0.9149 0.045 Uiso 1 1 calc R
C9 C 0.1459(2) 0.31363(14) 0.6779(3) 0.0351(7) Uani 1 1 d .
C10 C 0.0421(3) 0.31220(19) 0.5495(4) 0.0569(10) Uani 1 1 d .
H10A H 0.0301 0.3502 0.5014 0.085 Uiso 1 1 calc R
H10B H -0.0024 0.3103 0.5652 0.085 Uiso 1 1 calc R
H10C H 0.0336 0.2752 0.5013 0.085 Uiso 1 1 calc R
C11 C 0.1622(3) 0.37386(17) 0.7537(4) 0.0507(9) Uani 1 1 d .
H11A H 0.2288 0.3758 0.8313 0.076 Uiso 1 1 calc R
H11B H 0.1211 0.3725 0.7752 0.076 Uiso 1 1 calc R
H11C H 0.1469 0.4110 0.7022 0.076 Uiso 1 1 calc R
C12 C 0.2179(2) 0.30940(14) 0.6552(3) 0.0321(7) Uani 1 1 d .
C13 C 0.2330(2) 0.35272(14) 0.5936(3) 0.0345(7) Uani 1 1 d .
H13 H 0.1969 0.3902 0.5586 0.041 Uiso 1 1 calc R
C14 C 0.3034(2) 0.33901(14) 0.5853(3) 0.0319(7) Uani 1 1 d .
C15 C 0.3585(2) 0.28385(15) 0.6371(3) 0.0364(7) Uani 1 1 d .
H15 H 0.4056 0.2761 0.6302 0.044 Uiso 1 1 calc R
C16 C 0.3437(2) 0.24009(14) 0.6992(3) 0.0349(7) Uani 1 1 d .
H16 H 0.3803 0.2028 0.7342 0.042 Uiso 1 1 calc R
C17 C 0.2729(2) 0.25324(14) 0.7079(3) 0.0310(7) Uani 1 1 d .
C18 C 0.2969(2) 0.45343(15) 0.3967(3) 0.0407(8) Uani 1 1 d .
H18 H 0.2662 0.4818 0.3279 0.049 Uiso 1 1 calc R
C19 C 0.4069(2) 0.40289(14) 0.5627(3) 0.0323(7) Uani 1 1 d .
H19 H 0.4669 0.3878 0.6352 0.039 Uiso 1 1 calc R
Cl1 Cl 0.11349(6) 0.02162(4) 1.22923(7) 0.0375(2) Uani 1 1 d .
N1 N 0.05222(18) 0.08209(11) 0.9699(2) 0.0305(6) Uani 1 1 d .
N2 N 0.0959(2) 0.18377(11) 0.9755(3) 0.0422(7) Uani 1 1 d .
N3 N 0.11334(18) 0.14514(11) 0.9119(2) 0.0311(6) Uani 1 1 d .
N4 N 0.32146(18) 0.38351(11) 0.5238(2) 0.0329(6) Uani 1 1 d .
N5 N 0.2487(2) 0.41694(13) 0.4171(3) 0.0436(7) Uani 1 1 d .
N6 N 0.39389(18) 0.44655(11) 0.4830(2) 0.0306(6) Uani 1 1 d .
Ni1 Ni 0.0000 0.0000 1.0000 0.02544(17) Uani 1 2 d S
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'
Cl Cl 0.1484 0.1585 '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
N2 C1 N1 115.7(3) . .
N2 C1 H1 122.1 . .
N1 C1 H1 122.1 . .
N1 C2 N3 110.0(3) . .
N1 C2 H2 125.0 . .
N3 C2 H2 125.0 . .
C8 C3 C4 122.1(3) . .
C8 C3 N3 119.0(3) . .
C4 C3 N3 118.9(3) . .
C5 C4 C3 117.9(3) . .
C5 C4 H4 121.0 . .
C3 C4 H4 121.0 . .
C4 C5 C6 120.6(3) . .
C4 C5 C9 128.1(3) . .
C6 C5 C9 111.3(2) . .
C7 C6 C5 120.5(3) . .
C7 C6 C17 131.2(3) . .
C5 C6 C17 108.3(3) . .
C6 C7 C8 119.2(3) . .
C6 C7 H7 120.4 . .
C8 C7 H7 120.4 . .
C3 C8 C7 119.6(3) . .
C3 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C5 C9 C12 100.8(2) . .
C5 C9 C10 110.9(3) . .
C12 C9 C10 110.2(3) . .
C5 C9 C11 112.9(3) . .
C12 C9 C11 111.6(3) . .
C10 C9 C11 110.2(3) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C13 C12 C17 120.5(3) . .
C13 C12 C9 128.3(3) . .
C17 C12 C9 111.2(3) . .
C12 C13 C14 118.2(3) . .
C12 C13 H13 120.9 . .
C14 C13 H13 120.9 . .
C13 C14 C15 122.0(3) . .
C13 C14 N4 119.2(3) . .
C15 C14 N4 118.7(3) . .
C14 C15 C16 120.2(3) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C15 C16 C17 118.4(3) . .
C15 C16 H16 120.8 . .
C17 C16 H16 120.8 . .
C16 C17 C12 120.8(3) . .
C16 C17 C6 130.9(3) . .
C12 C17 C6 108.3(3) . .
N5 C18 N6 114.9(3) . .
N5 C18 H18 122.5 . .
N6 C18 H18 122.5 . .
N6 C19 N4 109.9(3) . .
N6 C19 H19 125.0 . .
N4 C19 H19 125.0 . .
C2 N1 C1 102.7(2) . .
C2 N1 Ni1 127.68(19) . .
C1 N1 Ni1 129.6(2) . .
C1 N2 N3 101.5(2) . .
C2 N3 N2 110.0(2) . .
C2 N3 C3 129.3(3) . .
N2 N3 C3 120.6(2) . .
C19 N4 N5 109.8(2) . .
C19 N4 C14 127.9(3) . .
N5 N4 C14 122.1(3) . .
C18 N5 N4 102.0(3) . .
C19 N6 C18 103.3(2) . .
C19 N6 Ni1 127.9(2) . 4_556
C18 N6 Ni1 128.5(2) . 4_556
N6 Ni1 N6 180.00(15) 4_546 8_456
N6 Ni1 N1 87.78(10) 4_546 .
N6 Ni1 N1 92.22(10) 8_456 .
N6 Ni1 N1 92.22(10) 4_546 5_557
N6 Ni1 N1 87.78(10) 8_456 5_557
N1 Ni1 N1 180.00(16) . 5_557
N6 Ni1 Cl1 89.68(8) 4_546 5_557
N6 Ni1 Cl1 90.32(8) 8_456 5_557
N1 Ni1 Cl1 90.76(8) . 5_557
N1 Ni1 Cl1 89.24(8) 5_557 5_557
N6 Ni1 Cl1 90.32(8) 4_546 .
N6 Ni1 Cl1 89.68(8) 8_456 .
N1 Ni1 Cl1 89.24(8) . .
N1 Ni1 Cl1 90.76(8) 5_557 .
Cl1 Ni1 Cl1 180.0 5_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.312(4) .
C1 N1 1.347(4) .
C1 H1 0.9300 .
C2 N1 1.317(4) .
C2 N3 1.334(4) .
C2 H2 0.9300 .
C3 C8 1.383(4) .
C3 C4 1.386(4) .
C3 N3 1.433(4) .
C4 C5 1.380(4) .
C4 H4 0.9300 .
C5 C6 1.400(4) .
C5 C9 1.522(4) .
C6 C7 1.383(4) .
C6 C17 1.466(4) .
C7 C8 1.385(4) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 C12 1.524(4) .
C9 C10 1.527(5) .
C9 C11 1.531(5) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 C13 1.377(4) .
C12 C17 1.399(4) .
C13 C14 1.380(4) .
C13 H13 0.9300 .
C14 C15 1.381(4) .
C14 N4 1.423(3) .
C15 C16 1.384(4) .
C15 H15 0.9300 .
C16 C17 1.389(4) .
C16 H16 0.9300 .
C18 N5 1.315(4) .
C18 N6 1.346(4) .
C18 H18 0.9300 .
C19 N6 1.317(4) .
C19 N4 1.333(4) .
C19 H19 0.9300 .
Cl1 Ni1 2.4225(19) .
N1 Ni1 2.123(2) .
N2 N3 1.362(3) .
N4 N5 1.363(4) .
N6 Ni1 2.101(3) 4_556
Ni1 N6 2.101(3) 4_546
Ni1 N6 2.101(3) 8_456
Ni1 N1 2.123(2) 5_557
Ni1 Cl1 2.4225(19) 5_557
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
_geom_torsion_site_symmetry_4
C8 C3 C4 C5 1.7(5) .
N3 C3 C4 C5 -178.3(3) .
C3 C4 C5 C6 -2.0(4) .
C3 C4 C5 C9 176.0(3) .
C4 C5 C6 C7 0.8(4) .
C9 C5 C6 C7 -177.5(3) .
C4 C5 C6 C17 -178.1(3) .
C9 C5 C6 C17 3.5(3) .
C5 C6 C7 C8 0.8(4) .
C17 C6 C7 C8 179.5(3) .
C4 C3 C8 C7 -0.1(5) .
N3 C3 C8 C7 179.8(3) .
C6 C7 C8 C3 -1.2(5) .
C4 C5 C9 C12 179.0(3) .
C6 C5 C9 C12 -2.8(3) .
C4 C5 C9 C10 -64.4(4) .
C6 C5 C9 C10 113.8(3) .
C4 C5 C9 C11 59.9(4) .
C6 C5 C9 C11 -122.0(3) .
C5 C9 C12 C13 -178.2(3) .
C10 C9 C12 C13 64.6(4) .
C11 C9 C12 C13 -58.2(4) .
C5 C9 C12 C17 1.1(3) .
C10 C9 C12 C17 -116.1(3) .
C11 C9 C12 C17 121.1(3) .
C17 C12 C13 C14 0.2(4) .
C9 C12 C13 C14 179.4(3) .
C12 C13 C14 C15 -0.3(4) .
C12 C13 C14 N4 -179.0(3) .
C13 C14 C15 C16 0.3(5) .
N4 C14 C15 C16 179.0(3) .
C14 C15 C16 C17 -0.1(4) .
C15 C16 C17 C12 0.0(4) .
C15 C16 C17 C6 179.6(3) .
C13 C12 C17 C16 0.0(4) .
C9 C12 C17 C16 -179.4(3) .
C13 C12 C17 C6 -179.7(3) .
C9 C12 C17 C6 0.9(3) .
C7 C6 C17 C16 -1.2(5) .
C5 C6 C17 C16 177.6(3) .
C7 C6 C17 C12 178.4(3) .
C5 C6 C17 C12 -2.8(3) .
N3 C2 N1 C1 -0.4(3) .
N3 C2 N1 Ni1 -179.43(19) .
N2 C1 N1 C2 0.4(4) .
N2 C1 N1 Ni1 179.5(2) .
N1 C1 N2 N3 -0.3(4) .
N1 C2 N3 N2 0.2(4) .
N1 C2 N3 C3 177.9(3) .
C1 N2 N3 C2 0.0(3) .
C1 N2 N3 C3 -177.8(3) .
C8 C3 N3 C2 -38.6(5) .
C4 C3 N3 C2 141.4(3) .
C8 C3 N3 N2 138.8(3) .
C4 C3 N3 N2 -41.2(4) .
N6 C19 N4 N5 -2.2(3) .
N6 C19 N4 C14 -177.2(3) .
C13 C14 N4 C19 136.6(3) .
C15 C14 N4 C19 -42.2(4) .
C13 C14 N4 N5 -37.9(4) .
C15 C14 N4 N5 143.3(3) .
N6 C18 N5 N4 -1.1(4) .
C19 N4 N5 C18 1.9(3) .
C14 N4 N5 C18 177.3(3) .
N4 C19 N6 C18 1.4(3) .
N4 C19 N6 Ni1 174.95(18) 4_556
N5 C18 N6 C19 -0.2(4) .
N5 C18 N6 Ni1 -173.7(2) 4_556
C2 N1 Ni1 N6 34.4(3) 4_546
C1 N1 Ni1 N6 -144.4(3) 4_546
C2 N1 Ni1 N6 -145.6(3) 8_456
C1 N1 Ni1 N6 35.6(3) 8_456
C2 N1 Ni1 N1 -145(18) 5_557
C1 N1 Ni1 N1 36(18) 5_557
C2 N1 Ni1 Cl1 -55.3(3) 5_557
C1 N1 Ni1 Cl1 126.0(3) 5_557
C2 N1 Ni1 Cl1 124.7(3) .
C1 N1 Ni1 Cl1 -54.0(3) .
