#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:47:55 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179674 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/26/4512616.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_4512616
loop_
_publ_author_name
'Zheng, Sheng-Run'
'Pan, Mei'
'Wu, Kai'
'Chen, Ling'
'Jiang, Ji-Jun'
'Wang, Da-Wei'
'Shi, Jian-Ying'
'Su, Cheng-Yong'
_publ_section_title
;
 Assembly of Binuclear, Tetranuclear, and Multinuclear Complexes from
 Pincer-Like Mononuclear Metallotectons: Structural Diversity Dependent on
 Precursors
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              625
_journal_paper_doi               10.1021/cg501306n
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C32 H34 Cl2 N8 Ni O9'
_chemical_formula_weight         804.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.307(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5631(4)
_cell_length_b                   17.4706(6)
_cell_length_c                   17.6941(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3527.4(2)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13536
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.8936
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.555
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1117P)²+5.2329P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                5821
_reflns_number_total             6830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501306n_si_001.cif
_cod_data_source_block           complex7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4512610--4512617.cif.
;
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               4512616
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ni1 Ni 0.70706(4) 0.76860(3) 0.45121(3) 0.03255(17) Uani 1 1 d .
Cl1 Cl 0.84837(8) 0.47849(5) 0.32145(5) 0.0331(2) Uani 1 1 d .
C16 C 1.0329(3) 0.75003(19) 0.61218(17) 0.0250(6) Uani 1 1 d .
C27 C 1.0110(3) 0.76784(17) 0.17862(17) 0.0210(6) Uani 1 1 d .
Cl2 Cl 0.77388(9) 0.96080(6) 0.76167(5) 0.0426(3) Uani 1 1 d .
N5 N 0.8654(2) 0.75974(14) 0.52554(14) 0.0188(5) Uani 1 1 d .
N3 N 0.5584(2) 0.75970(15) 0.36772(14) 0.0199(5) Uani 1 1 d .
N8 N 1.1146(2) 0.74256(14) 0.04766(14) 0.0206(5) Uani 1 1 d .
N2 N 0.5228(2) 0.96332(15) 0.37786(15) 0.0220(5) Uani 1 1 d .
H2B H 0.4660 0.9794 0.3441 0.026 Uiso 1 1 calc R
N7 N 0.8145(2) 0.77792(14) 0.36362(14) 0.0193(5) Uani 1 1 d .
O3 O 0.9347(2) 0.43106(15) 0.29238(14) 0.0378(6) Uani 1 1 d .
N1 N 0.6514(2) 0.88332(14) 0.44401(13) 0.0184(5) Uani 1 1 d .
C28 C 1.1149(3) 0.72624(18) 0.18252(17) 0.0218(6) Uani 1 1 d .
H28A H 1.1514 0.7060 0.2289 0.026 Uiso 1 1 calc R
N4 N 0.7213(2) 0.64923(14) 0.46403(14) 0.0204(5) Uani 1 1 d .
O2 O 0.7674(3) 0.5074(2) 0.2584(2) 0.0621(10) Uani 1 1 d .
C26 C 0.8751(3) 0.71511(18) 0.34945(18) 0.0246(6) Uani 1 1 d .
H26A H 0.8717 0.6723 0.3802 0.029 Uiso 1 1 calc R
C25 C 0.9422(3) 0.71094(18) 0.29176(18) 0.0241(6) Uani 1 1 d .
H25A H 0.9814 0.6660 0.2837 0.029 Uiso 1 1 calc R
C29 C 1.1630(3) 0.71538(18) 0.11674(17) 0.0225(6) Uani 1 1 d .
H29A H 1.2324 0.6878 0.1204 0.027 Uiso 1 1 calc R
C24 C 0.9504(3) 0.77467(17) 0.24586(17) 0.0206(6) Uani 1 1 d .
C31 C 0.9608(3) 0.79672(19) 0.10765(18) 0.0255(6) Uani 1 1 d .
H31A H 0.8921 0.8253 0.1027 0.031 Uiso 1 1 calc R
O8 O 0.8338(3) 0.91288(19) 0.71534(15) 0.0478(7) Uani 1 1 d .
N6 N 0.9777(2) 0.68003(16) 0.60392(15) 0.0273(6) Uani 1 1 d .
H6A H 1.0012 0.6386 0.6278 0.033 Uiso 1 1 calc R
C30 C 1.0142(3) 0.78249(18) 0.04439(17) 0.0233(6) Uani 1 1 d .
H30A H 0.9789 0.8015 -0.0028 0.028 Uiso 1 1 calc R
O1 O 0.9063(3) 0.53894(17) 0.3672(2) 0.0530(8) Uani 1 1 d .
C23 C 0.8930(3) 0.84122(18) 0.26240(18) 0.0244(6) Uani 1 1 d .
H23A H 0.8993 0.8857 0.2345 0.029 Uiso 1 1 calc R
C1 C 0.6712(2) 0.95616(17) 0.47437(16) 0.0192(6) Uani 1 1 d .
C9 C 0.5057(2) 0.82304(18) 0.34721(16) 0.0209(6) Uani 1 1 d .
C2 C 0.7479(3) 0.98238(18) 0.53881(17) 0.0225(6) Uani 1 1 d .
H2A H 0.7989 0.9492 0.5689 0.027 Uiso 1 1 calc R
C21 C 0.9625(2) 0.79998(18) 0.56161(16) 0.0203(6) Uani 1 1 d .
C20 C 0.9985(3) 0.87548(19) 0.55290(18) 0.0250(6) Uani 1 1 d .
H20A H 0.9546 0.9088 0.5186 0.030 Uiso 1 1 calc R
C7 C 0.5603(2) 0.89035(17) 0.38776(16) 0.0199(6) Uani 1 1 d .
C5 C 0.5900(3) 1.08576(18) 0.44877(19) 0.0267(6) Uani 1 1 d .
H5A H 0.5381 1.1191 0.4196 0.032 Uiso 1 1 calc R
C10 C 0.5094(3) 0.68810(19) 0.33239(18) 0.0261(6) Uani 1 1 d .
H10A H 0.4828 0.6971 0.2783 0.031 Uiso 1 1 calc R
H10B H 0.4415 0.6740 0.3552 0.031 Uiso 1 1 calc R
C22 C 0.8263(3) 0.84048(17) 0.32103(17) 0.0225(6) Uani 1 1 d .
H22A H 0.7881 0.8852 0.3313 0.027 Uiso 1 1 calc R
C6 C 0.5924(3) 1.00744(17) 0.43198(17) 0.0215(6) Uani 1 1 d .
C15 C 0.8800(3) 0.68822(18) 0.55147(16) 0.0218(6) Uani 1 1 d .
C8 C 0.3941(3) 0.8312(2) 0.29206(19) 0.0296(7) Uani 1 1 d .
H8A H 0.3705 0.7822 0.2705 0.044 Uiso 1 1 calc R
H8B H 0.4058 0.8659 0.2518 0.044 Uiso 1 1 calc R
H8C H 0.3341 0.8510 0.3184 0.044 Uiso 1 1 calc R
C3 C 0.7448(3) 1.05970(19) 0.55583(19) 0.0279(7) Uani 1 1 d .
H3A H 0.7944 1.0785 0.5984 0.033 Uiso 1 1 calc R
C17 C 1.1374(3) 0.7735(2) 0.65709(19) 0.0325(7) Uani 1 1 d .
H17A H 1.1827 0.7403 0.6907 0.039 Uiso 1 1 calc R
C14 C 0.8003(3) 0.62658(17) 0.51937(17) 0.0238(6) Uani 1 1 d .
C11 C 0.5950(3) 0.62137(19) 0.34107(18) 0.0270(6) Uani 1 1 d .
H11A H 0.5580 0.5785 0.3118 0.032 Uiso 1 1 calc R
H11B H 0.6628 0.6360 0.3184 0.032 Uiso 1 1 calc R
C4 C 0.6683(3) 1.11070(19) 0.5104(2) 0.0295(7) Uani 1 1 d .
H4A H 0.6711 1.1625 0.5226 0.035 Uiso 1 1 calc R
C12 C 0.6378(3) 0.59421(18) 0.42248(19) 0.0260(6) Uani 1 1 d .
H12A H 0.5714 0.5883 0.4492 0.031 Uiso 1 1 calc R
H12B H 0.6755 0.5447 0.4211 0.031 Uiso 1 1 calc R
C19 C 1.1026(3) 0.8987(2) 0.5977(2) 0.0306(7) Uani 1 1 d .
H19A H 1.1283 0.9487 0.5935 0.037 Uiso 1 1 calc R
O4 O 0.7874(3) 0.43110(17) 0.36881(18) 0.0481(7) Uani 1 1 d .
O7 O 0.6510(3) 0.9622(2) 0.7309(2) 0.0649(10) Uani 1 1 d .
C18 C 1.1698(3) 0.8484(2) 0.64908(19) 0.0333(7) Uani 1 1 d .
H18A H 1.2384 0.8663 0.6786 0.040 Uiso 1 1 calc R
C13 C 0.8183(4) 0.5469(2) 0.5501(2) 0.0382(8) Uani 1 1 d .
H13A H 0.7593 0.5138 0.5231 0.057 Uiso 1 1 calc R
H13B H 0.8127 0.5468 0.6037 0.057 Uiso 1 1 calc R
H13C H 0.8944 0.5290 0.5432 0.057 Uiso 1 1 calc R
O6 O 0.7908(4) 0.9301(3) 0.83712(19) 0.0958(19) Uani 1 1 d .
O5 O 0.8178(4) 1.0369(2) 0.7626(3) 0.0892(15) Uani 1 1 d .
O9 O 0.7462(6) 0.7971(4) 0.9086(5) 0.121(2) Uani 1 1 d .
H9 H 0.7429 0.8356 0.8818 0.181 Uiso 1 1 calc R
C32 C 0.6715(8) 0.8051(7) 0.9612(5) 0.113(3) Uani 1 1 d .
H32A H 0.7163 0.8139 1.0110 0.169 Uiso 1 1 calc R
H32B H 0.6260 0.7593 0.9622 0.169 Uiso 1 1 calc R
H32C H 0.6201 0.8477 0.9471 0.169 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'
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_3
N5 Ni1 N3 169.66(10) .
N5 Ni1 N4 79.17(10) .
N3 Ni1 N4 92.52(10) .
N5 Ni1 N1 109.80(10) .
N3 Ni1 N1 79.56(10) .
N4 Ni1 N1 166.05(9) .
N5 Ni1 N7 84.80(9) .
N3 Ni1 N7 90.06(10) .
N4 Ni1 N7 96.25(9) .
N1 Ni1 N7 95.23(9) .
N5 Ni1 N8 89.48(10) 4_576
N3 Ni1 N8 95.53(10) 4_576
N4 Ni1 N8 82.28(9) 4_576
N1 Ni1 N8 87.04(9) 4_576
N7 Ni1 N8 174.27(10) 4_576
O2 Cl1 O1 111.7(2) .
O2 Cl1 O4 109.7(2) .
O1 Cl1 O4 108.86(19) .
O2 Cl1 O3 108.99(18) .
O1 Cl1 O3 109.63(19) .
O4 Cl1 O3 107.86(17) .
N6 C16 C17 131.7(3) .
N6 C16 C21 105.8(3) .
C17 C16 C21 122.5(3) .
C31 C27 C28 117.6(3) .
C31 C27 C24 121.0(3) .
C28 C27 C24 121.2(3) .
O6 Cl2 O5 110.3(3) .
O6 Cl2 O8 108.17(19) .
O5 Cl2 O8 110.4(3) .
O6 Cl2 O7 109.8(3) .
O5 Cl2 O7 108.6(2) .
O8 Cl2 O7 109.5(2) .
C15 N5 C21 105.6(2) .
C15 N5 Ni1 109.7(2) .
C21 N5 Ni1 144.7(2) .
C9 N3 C10 118.6(3) .
C9 N3 Ni1 115.8(2) .
C10 N3 Ni1 125.6(2) .
C29 N8 C30 116.7(3) .
C29 N8 Ni1 119.9(2) 4_675
C30 N8 Ni1 123.0(2) 4_675
C7 N2 C6 107.3(2) .
C26 N7 C22 117.0(3) .
C26 N7 Ni1 116.9(2) .
C22 N7 Ni1 126.1(2) .
C7 N1 C1 105.4(2) .
C7 N1 Ni1 109.28(19) .
C1 N1 Ni1 145.3(2) .
C29 C28 C27 119.3(3) .
C14 N4 C12 120.4(3) .
C14 N4 Ni1 114.9(2) .
C12 N4 Ni1 124.1(2) .
N7 C26 C25 123.5(3) .
C26 C25 C24 119.3(3) .
N8 C29 C28 123.5(3) .
C25 C24 C23 117.7(3) .
C25 C24 C27 119.4(3) .
C23 C24 C27 122.7(3) .
C30 C31 C27 119.3(3) .
C15 N6 C16 107.5(3) .
N8 C30 C31 123.5(3) .
C22 C23 C24 119.3(3) .
N1 C1 C6 109.1(3) .
N1 C1 C2 131.1(3) .
C6 C1 C2 119.7(3) .
N3 C9 C7 113.9(3) .
N3 C9 C8 125.9(3) .
C7 C9 C8 120.1(3) .
C3 C2 C1 117.3(3) .
N5 C21 C20 131.2(3) .
N5 C21 C16 108.6(3) .
C20 C21 C16 120.1(3) .
C19 C20 C21 117.2(3) .
N1 C7 N2 112.5(3) .
N1 C7 C9 121.2(3) .
N2 C7 C9 126.2(3) .
C4 C5 C6 116.5(3) .
N3 C10 C11 114.1(3) .
N7 C22 C23 123.0(3) .
N2 C6 C1 105.6(3) .
N2 C6 C5 131.5(3) .
C1 C6 C5 122.9(3) .
N5 C15 N6 112.5(3) .
N5 C15 C14 121.1(3) .
N6 C15 C14 126.2(3) .
C2 C3 C4 121.9(3) .
C18 C17 C16 116.5(3) .
N4 C14 C15 113.0(3) .
N4 C14 C13 127.0(3) .
C15 C14 C13 119.9(3) .
C12 C11 C10 116.2(3) .
C5 C4 C3 121.6(3) .
N4 C12 C11 110.8(3) .
C20 C19 C18 121.6(3) .
C17 C18 C19 122.0(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N5 2.080(2) .
Ni1 N3 2.083(2) .
Ni1 N4 2.101(3) .
Ni1 N1 2.103(2) .
Ni1 N7 2.143(2) .
Ni1 N8 2.164(2) 4_576
Cl1 O2 1.428(3) .
Cl1 O1 1.430(3) .
Cl1 O4 1.440(3) .
Cl1 O3 1.454(3) .
C16 N6 1.376(4) .
C16 C17 1.396(5) .
C16 C21 1.410(4) .
C27 C31 1.390(4) .
C27 C28 1.396(4) .
C27 C24 1.480(4) .
Cl2 O6 1.423(3) .
Cl2 O5 1.422(5) .
Cl2 O8 1.427(3) .
Cl2 O7 1.437(4) .
N5 C15 1.332(4) .
N5 C21 1.390(4) .
N3 C9 1.287(4) .
N3 C10 1.470(4) .
N8 C29 1.346(4) .
N8 C30 1.348(4) .
N8 Ni1 2.164(2) 4_675
N2 C7 1.349(4) .
N2 C6 1.382(4) .
N7 C26 1.348(4) .
N7 C22 1.347(4) .
N1 C7 1.333(4) .
N1 C1 1.386(4) .
C28 C29 1.382(4) .
N4 C14 1.288(4) .
N4 C12 1.472(4) .
C26 C25 1.380(4) .
C25 C24 1.391(4) .
C24 C23 1.393(4) .
C31 C30 1.385(4) .
N6 C15 1.349(4) .
C23 C22 1.389(4) .
C1 C6 1.405(4) .
C1 C2 1.404(4) .
C9 C7 1.466(4) .
C9 C8 1.494(4) .
C2 C3 1.386(5) .
C21 C20 1.399(4) .
C20 C19 1.390(5) .
C5 C4 1.371(5) .
C5 C6 1.401(4) .
C10 C11 1.521(4) .
C15 C14 1.470(4) .
C3 C4 1.411(5) .
C17 C18 1.374(6) .
C14 C13 1.497(4) .
C11 C12 1.521(5) .
C19 C18 1.406(5) .
O9 C32 1.375(9) .
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
N2 H2B O7 0.86 2.01 2.861(4) 168.4 3_676
N6 H6A O3 0.86 1.92 2.749(4) 161.7 3_766
O9 H9 O6 0.82 1.95 2.734(8) 159.9 .
