#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:22:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180036 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/30/7033073.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_7033073
loop_
_publ_author_name
'Ohno, Keiji'
'Nagasawa, Akira'
'Fujihara, Takashi'
_publ_section_title
;
 Dinuclear nickel(II) complexes with 2,5-diamino-1,4-benzoquinonediimine
 ligands as precatalysts for the polymerization of styrene: electronic and
 steric substituent effects.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              368
_journal_page_last               376
_journal_paper_doi               10.1039/c4dt02858a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C50 H54 Cl6 N4 Ni2 O8'
_chemical_formula_weight         1169.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.63(3)
_cell_angle_beta                 109.84(3)
_cell_angle_gamma                91.01(3)
_cell_formula_units_Z            1
_cell_length_a                   10.747(2)
_cell_length_b                   11.215(2)
_cell_length_c                   12.347(3)
_cell_measurement_reflns_used    2202
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1352.6(6)
_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      173(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9834
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.9495
_exptl_absorpt_correction_T_min  0.8340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0703
_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)+(0.1055P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2028
_reflns_number_gt                3852
_reflns_number_total             6418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02858a2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 2827 2014-09-09 07:05:25Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

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

 Adding full bibliography for 7033073--7033079.cif.
;
_cod_original_cell_volume        1352.5(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7033073
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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
C1 C 0.8903(4) 0.9194(4) 0.9114(4) 0.0237(9) Uani 1 1 d .
C2 C 0.9544(4) 1.0220(4) 0.8851(4) 0.0245(9) Uani 1 1 d .
C3 C 1.0613(4) 1.0998(4) 0.9738(4) 0.0259(9) Uani 1 1 d .
H3 H 1.1005 1.1644 0.9571 0.031 Uiso 1 1 calc R
C4 C 0.7231(4) 0.7473(4) 0.8265(4) 0.0277(9) Uani 1 1 d .
C5 C 0.7901(4) 0.6452(4) 0.8447(4) 0.0339(10) Uani 1 1 d .
H5 H 0.8793 0.6465 0.8524 0.041 Uiso 1 1 calc R
C6 C 0.7246(5) 0.5410(4) 0.8516(4) 0.0356(11) Uani 1 1 d .
H6 H 0.7702 0.4731 0.8651 0.043 Uiso 1 1 calc R
C7 C 0.5913(4) 0.5382(4) 0.8382(4) 0.0312(10) Uani 1 1 d .
C8 C 0.5240(4) 0.6402(4) 0.8193(4) 0.0342(10) Uani 1 1 d .
H8 H 0.4343 0.6387 0.8100 0.041 Uiso 1 1 calc R
C9 C 0.5910(4) 0.7443(4) 0.8145(4) 0.0322(10) Uani 1 1 d .
H9 H 0.5462 0.8130 0.8030 0.039 Uiso 1 1 calc R
C10 C 0.4007(5) 0.4280(5) 0.8441(4) 0.0404(12) Uani 1 1 d .
H10A H 0.3411 0.4403 0.7694 0.049 Uiso 1 1 calc R
H10B H 0.3944 0.4931 0.9088 0.049 Uiso 1 1 calc R
C11 C 0.3635(5) 0.3037(5) 0.8579(5) 0.0493(14) Uani 1 1 d .
H11A H 0.3627 0.2405 0.7899 0.074 Uiso 1 1 calc R
H11B H 0.2768 0.3017 0.8640 0.074 Uiso 1 1 calc R
H11C H 0.4274 0.2897 0.9287 0.074 Uiso 1 1 calc R
C12 C 0.9506(4) 1.1182(4) 0.7318(4) 0.0268(9) Uani 1 1 d .
C13 C 0.9258(5) 1.2401(4) 0.7605(4) 0.0358(11) Uani 1 1 d .
H13 H 0.8777 1.2647 0.8104 0.043 Uiso 1 1 calc R
C14 C 0.9727(5) 1.3256(4) 0.7151(5) 0.0407(12) Uani 1 1 d .
H14 H 0.9567 1.4077 0.7351 0.049 Uiso 1 1 calc R
C15 C 1.0430(4) 1.2895(4) 0.6402(4) 0.0308(10) Uani 1 1 d .
C16 C 1.0668(4) 1.1686(4) 0.6106(4) 0.0315(10) Uani 1 1 d .
H16 H 1.1139 1.1439 0.5598 0.038 Uiso 1 1 calc R
C17 C 1.0202(4) 1.0831(4) 0.6568(4) 0.0310(10) Uani 1 1 d .
H17 H 1.0363 1.0011 0.6367 0.037 Uiso 1 1 calc R
C18 C 1.1562(5) 1.3466(5) 0.5201(5) 0.0387(11) Uani 1 1 d .
H18A H 1.0986 1.2891 0.4474 0.046 Uiso 1 1 calc R
H18B H 1.2337 1.3069 0.5555 0.046 Uiso 1 1 calc R
C19 C 1.1976(6) 1.4609(5) 0.4931(6) 0.0542(15) Uani 1 1 d .
H19A H 1.1202 1.4996 0.4584 0.081 Uiso 1 1 calc R
H19B H 1.2439 1.4397 0.4381 0.081 Uiso 1 1 calc R
H19C H 1.2553 1.5168 0.5654 0.081 Uiso 1 1 calc R
C20 C 0.5322(5) 0.7728(5) 0.4907(4) 0.0358(11) Uani 1 1 d .
C21 C 0.5351(4) 0.8472(4) 0.4169(4) 0.0347(11) Uani 1 1 d .
H21 H 0.4687 0.8317 0.3421 0.042 Uiso 1 1 calc R
C22 C 0.6343(4) 0.9454(4) 0.4504(4) 0.0304(10) Uani 1 1 d .
C23 C 0.4272(5) 0.6659(5) 0.4491(5) 0.0485(14) Uani 1 1 d .
H23A H 0.4563 0.5944 0.4083 0.073 Uiso 1 1 calc R
H23B H 0.3463 0.6854 0.3959 0.073 Uiso 1 1 calc R
H23C H 0.4115 0.6494 0.5166 0.073 Uiso 1 1 calc R
C24 C 0.6352(5) 1.0196(5) 0.3649(4) 0.0406(12) Uani 1 1 d .
H24A H 0.6592 1.1052 0.4070 0.061 Uiso 1 1 calc R
H24B H 0.5482 1.0096 0.3049 0.061 Uiso 1 1 calc R
H24C H 0.6986 0.9919 0.3280 0.061 Uiso 1 1 calc R
C25 C 0.7914(7) 0.1826(7) 0.0976(7) 0.076(2) Uani 1 1 d .
H25 H 0.8650 0.1399 0.0825 0.092 Uiso 1 1 calc R
Cl1 Cl 0.7259(3) 0.2595(3) -0.0098(3) 0.1431(12) Uani 1 1 d .
Cl2 Cl 0.8475(3) 0.2746(5) 0.2365(3) 0.235(3) Uani 1 1 d .
Cl3 Cl 0.6690(3) 0.0739(3) 0.0875(4) 0.1541(14) Uani 1 1 d .
N1 N 0.7906(3) 0.8537(3) 0.8178(3) 0.0270(8) Uani 1 1 d .
N2 N 0.8986(3) 1.0272(3) 0.7730(3) 0.0253(8) Uani 1 1 d .
Ni1 Ni 0.75297(5) 0.90864(5) 0.67783(5) 0.02686(19) Uani 1 1 d .
O1 O 0.5345(3) 0.4303(3) 0.8456(3) 0.0387(8) Uani 1 1 d .
O2 O 1.0873(3) 1.3818(3) 0.6010(3) 0.0395(8) Uani 1 1 d .
O3 O 0.6145(3) 0.7856(3) 0.5957(3) 0.0327(7) Uani 1 1 d .
O4 O 0.7278(3) 0.9768(3) 0.5507(3) 0.0310(7) Uani 1 1 d .
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_1
_geom_angle_site_symmetry_3
N1 C1 C3 127.3(4) . 2_777
N1 C1 C2 113.1(4) . .
C3 C1 C2 119.6(4) 2_777 .
N2 C2 C3 127.1(4) . .
N2 C2 C1 112.5(4) . .
C3 C2 C1 120.4(4) . .
C2 C3 C1 119.9(4) . 2_777
C2 C3 H3 120.0 . .
C1 C3 H3 120.0 2_777 .
C9 C4 C5 119.5(4) . .
C9 C4 N1 120.5(4) . .
C5 C4 N1 120.0(4) . .
C4 C5 C6 120.2(4) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C7 C6 C5 119.9(4) . .
C7 C6 H6 120.0 . .
C5 C6 H6 120.0 . .
O1 C7 C6 115.7(4) . .
O1 C7 C8 124.4(4) . .
C6 C7 C8 119.9(4) . .
C9 C8 C7 119.6(4) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C4 C9 C8 120.8(4) . .
C4 C9 H9 119.6 . .
C8 C9 H9 119.6 . .
O1 C10 C11 107.5(4) . .
O1 C10 H10A 110.2 . .
C11 C10 H10A 110.2 . .
O1 C10 H10B 110.2 . .
C11 C10 H10B 110.2 . .
H10A C10 H10B 108.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C17 C12 C13 119.2(4) . .
C17 C12 N2 119.4(4) . .
C13 C12 N2 121.3(4) . .
C14 C13 C12 120.1(4) . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C14 C13 120.2(4) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C16 C15 C14 120.0(4) . .
C16 C15 O2 124.2(4) . .
C14 C15 O2 115.8(4) . .
C15 C16 C17 119.7(4) . .
C15 C16 H16 120.2 . .
C17 C16 H16 120.2 . .
C12 C17 C16 120.8(4) . .
C12 C17 H17 119.6 . .
C16 C17 H17 119.6 . .
O2 C18 C19 107.7(4) . .
O2 C18 H18A 110.2 . .
C19 C18 H18A 110.2 . .
O2 C18 H18B 110.2 . .
C19 C18 H18B 110.2 . .
H18A C18 H18B 108.5 . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O3 C20 C21 125.2(4) . .
O3 C20 C23 114.2(4) . .
C21 C20 C23 120.6(4) . .
C20 C21 C22 122.5(4) . .
C20 C21 H21 118.7 . .
C22 C21 H21 118.7 . .
O4 C22 C21 124.3(4) . .
O4 C22 C24 115.6(4) . .
C21 C22 C24 120.1(4) . .
C20 C23 H23A 109.5 . .
C20 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C20 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C22 C24 H24A 109.5 . .
C22 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C22 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
Cl2 C25 Cl1 113.6(5) . .
Cl2 C25 Cl3 108.4(5) . .
Cl1 C25 Cl3 108.4(4) . .
Cl2 C25 H25 108.8 . .
Cl1 C25 H25 108.8 . .
Cl3 C25 H25 108.8 . .
C1 N1 C4 120.0(4) . .
C1 N1 Ni1 115.2(3) . .
C4 N1 Ni1 124.8(3) . .
C2 N2 C12 119.8(4) . .
C2 N2 Ni1 115.7(3) . .
C12 N2 Ni1 124.5(3) . .
O3 Ni1 O4 94.41(13) . .
O3 Ni1 N2 174.82(14) . .
O4 Ni1 N2 90.72(14) . .
O3 Ni1 N1 91.37(14) . .
O4 Ni1 N1 174.09(14) . .
N2 Ni1 N1 83.51(15) . .
C7 O1 C10 117.5(4) . .
C15 O2 C18 117.2(4) . .
C20 O3 Ni1 126.4(3) . .
C22 O4 Ni1 126.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.325(5) .
C1 C3 1.405(6) 2_777
C1 C2 1.484(6) .
C2 N2 1.325(5) .
C2 C3 1.393(6) .
C3 C1 1.405(6) 2_777
C3 H3 0.9300 .
C4 C9 1.375(6) .
C4 C5 1.386(6) .
C4 N1 1.431(5) .
C5 C6 1.388(6) .
C5 H5 0.9300 .
C6 C7 1.385(6) .
C6 H6 0.9300 .
C7 O1 1.382(5) .
C7 C8 1.388(6) .
C8 C9 1.384(6) .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 O1 1.431(6) .
C10 C11 1.506(7) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 C17 1.371(6) .
C12 C13 1.384(6) .
C12 N2 1.424(5) .
C13 C14 1.384(6) .
C13 H13 0.9300 .
C14 C15 1.378(7) .
C14 H14 0.9300 .
C15 C16 1.371(6) .
C15 O2 1.381(5) .
C16 C17 1.390(6) .
C16 H16 0.9300 .
C17 H17 0.9300 .
C18 O2 1.425(6) .
C18 C19 1.494(7) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C20 O3 1.270(5) .
C20 C21 1.380(6) .
C20 C23 1.498(7) .
C21 C22 1.401(6) .
C21 H21 0.9300 .
C22 O4 1.267(5) .
C22 C24 1.492(6) .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 Cl2 1.677(9) .
C25 Cl1 1.710(7) .
C25 Cl3 1.729(8) .
C25 H25 0.9800 .
N1 Ni1 1.888(3) .
N2 Ni1 1.881(3) .
Ni1 O3 1.842(3) .
Ni1 O4 1.846(3) .
