#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:15:23 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179960 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/54/7025497.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_7025497
loop_
_publ_author_name
'Sgro, Michael J.'
'Stephan, Douglas W.'
_publ_section_title
;
 Synthesis and exchange reactions of Ni-dimine-COD, acetylene and olefin
 complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5786
_journal_page_last               5794
_journal_paper_doi               10.1039/c001312a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C72 H80 N4 Ni'
_chemical_formula_weight         1060.11
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.524(3)
_cell_length_b                   23.805(4)
_cell_length_c                   14.728(3)
_cell_measurement_reflns_used    4028
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.77
_cell_volume                     5793.3(19)
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11917
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6271
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0314
_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)+(0.0456P)²+3.6991P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                2131
_reflns_number_total             2558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001312a.txt
_cod_data_source_block           C72H80N4Ni_Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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        5793.2(16)
_cod_original_sg_symbol_H-M      Ccca
_cod_database_code               7025497
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x, 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 0.0000 0.2500 0.2500 0.02003(14) Uani 1 4 d S
N1 N 0.03180(8) 0.18847(5) 0.33082(9) 0.0223(3) Uani 1 1 d .
C1 C 0.05908(10) 0.18719(6) 0.42325(11) 0.0230(4) Uani 1 1 d .
C8 C 0.01624(9) 0.13874(7) 0.29494(11) 0.0233(4) Uani 1 1 d .
C6 C 0.14175(11) 0.18998(7) 0.44041(11) 0.0275(4) Uani 1 1 d .
C3 C 0.03282(12) 0.17887(7) 0.58206(12) 0.0312(4) Uani 1 1 d .
H3 H -0.0039 0.1760 0.6297 0.037 Uiso 1 1 calc R
C4 C 0.11424(12) 0.18136(8) 0.60166(12) 0.0336(4) Uani 1 1 d .
C2 C 0.00352(11) 0.18056(7) 0.49363(12) 0.0260(4) Uani 1 1 d .
C9 C 0.02664(11) 0.08058(7) 0.32448(12) 0.0280(4) Uani 1 1 d .
C5 C 0.16821(12) 0.18659(8) 0.53003(12) 0.0344(4) Uani 1 1 d .
H5 H 0.2234 0.1879 0.5421 0.041 Uiso 1 1 calc R
C7 C 0.20082(11) 0.19447(9) 0.36343(13) 0.0394(5) Uani 1 1 d .
H7A H 0.2545 0.1990 0.3872 0.059 Uiso 1 1 calc R
H7B H 0.1873 0.2264 0.3265 0.059 Uiso 1 1 calc R
H7C H 0.1984 0.1610 0.3273 0.059 Uiso 1 1 calc R
C10 C 0.05474(12) 0.05389(8) 0.40096(13) 0.0358(5) Uani 1 1 d .
H10 H 0.0729 0.0743 0.4508 0.043 Uiso 1 1 calc R
C14 C 0.0000 0.04772(10) 0.2500 0.0309(6) Uani 1 2 d S
C11 C 0.05527(14) -0.00547(9) 0.40156(14) 0.0474(6) Uani 1 1 d .
H11 H 0.0742 -0.0239 0.4530 0.057 Uiso 1 1 calc R
C12 C 0.02918(15) -0.03680(8) 0.32992(15) 0.0498(6) Uani 1 1 d .
H12 H 0.0305 -0.0758 0.3335 0.060 Uiso 1 1 calc R
C13 C 0.0000 -0.01066(11) 0.2500 0.0406(7) Uani 1 2 d S
C15 C 0.20862(17) 0.44648(12) 0.3517(2) 0.0792(9) Uani 1 1 d .
H15A H 0.1522 0.4577 0.3522 0.095 Uiso 1 1 calc R
H15B H 0.2107 0.4058 0.3516 0.095 Uiso 1 1 calc R
C16 C 0.2481(2) 0.46833(12) 0.2672(2) 0.0798(9) Uani 1 1 d .
H16A H 0.2179 0.4557 0.2145 0.096 Uiso 1 1 calc R
H16B H 0.3025 0.4533 0.2627 0.096 Uiso 1 1 calc R
C17 C 0.2491(2) 0.46802(13) 0.4350(2) 0.0894(10) Uani 1 1 d .
H17A H 0.3040 0.4537 0.4379 0.107 Uiso 1 1 calc R
H17B H 0.2202 0.4548 0.4883 0.107 Uiso 1 1 calc R
C18 C -0.08510(11) 0.17313(8) 0.47570(14) 0.0368(5) Uani 1 1 d .
H18A H -0.0964 0.1341 0.4650 0.055 Uiso 1 1 calc R
H18B H -0.1002 0.1946 0.4233 0.055 Uiso 1 1 calc R
H18C H -0.1154 0.1858 0.5274 0.055 Uiso 1 1 calc R
C19 C 0.14403(16) 0.17703(10) 0.69848(13) 0.0536(6) Uani 1 1 d .
H19A H 0.1435 0.1384 0.7172 0.080 Uiso 1 1 calc R
H19B H 0.1093 0.1985 0.7375 0.080 Uiso 1 1 calc R
H19C H 0.1982 0.1914 0.7022 0.080 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'
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 Ni1 N1 105.17(8) 8_455 3
N1 Ni1 N1 83.23(8) 8_455 6_455
N1 Ni1 N1 148.89(8) 3 6_455
N1 Ni1 N1 148.89(8) 8_455 .
N1 Ni1 N1 83.23(8) 3 .
N1 Ni1 N1 105.17(8) 6_455 .
C8 N1 C1 114.94(13) . .
C8 N1 Ni1 111.99(11) . .
C1 N1 Ni1 132.59(10) . .
C6 C1 C2 121.15(15) . .
C6 C1 N1 118.70(15) . .
C2 C1 N1 120.07(15) . .
N1 C8 C8 116.34(9) . 3
N1 C8 C9 134.96(15) . .
C8 C8 C9 108.67(10) 3 .
C1 C6 C5 118.54(16) . .
C1 C6 C7 120.35(15) . .
C5 C6 C7 121.07(16) . .
C4 C3 C2 122.38(17) . .
C3 C4 C5 118.20(16) . .
C3 C4 C19 120.85(18) . .
C5 C4 C19 120.94(19) . .
C3 C2 C1 118.07(17) . .
C3 C2 C18 120.14(16) . .
C1 C2 C18 121.74(16) . .
C10 C9 C14 118.96(17) . .
C10 C9 C8 136.22(17) . .
C14 C9 C8 104.82(16) . .
C4 C5 C6 121.61(18) . .
C9 C10 C11 118.01(19) . .
C13 C14 C9 123.49(11) . .
C13 C14 C9 123.49(11) . 3
C9 C14 C9 113.0(2) . 3
C12 C11 C10 122.7(2) . .
C11 C12 C13 120.72(19) . .
C14 C13 C12 116.07(13) . .
C14 C13 C12 116.07(13) . 3
C12 C13 C12 127.9(3) . 3
C17 C15 C16 111.7(2) . .
C15 C16 C16 111.4(2) . 2_565
C15 C17 C17 110.7(2) . 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.9592(13) 8_455
Ni1 N1 1.9592(13) 3
Ni1 N1 1.9592(13) 6_455
Ni1 N1 1.9592(13) .
N1 C8 1.322(2) .
N1 C1 1.434(2) .
C1 C6 1.391(2) .
C1 C2 1.394(2) .
C8 C8 1.428(3) 3
C8 C9 1.461(2) .
C6 C5 1.393(2) .
C6 C7 1.500(3) .
C3 C4 1.377(3) .
C3 C2 1.390(3) .
C4 C5 1.387(3) .
C4 C19 1.512(3) .
C2 C18 1.498(3) .
C9 C10 1.374(3) .
C9 C14 1.417(2) .
C10 C11 1.413(3) .
C14 C13 1.390(4) .
C14 C9 1.417(2) 3
C11 C12 1.362(3) .
C12 C13 1.416(2) .
C13 C12 1.416(2) 3
C15 C17 1.489(4) .
C15 C16 1.499(4) .
C16 C16 1.509(6) 2_565
C17 C17 1.523(6) 2_565
