#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:55:59 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178614 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/25/4072574.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_4072574
loop_
_publ_author_name
'Meinhard, Dieter'
'Reuter, Peter'
'Rieger, Bernhard'
_publ_section_title
;
 Activation of Polymerization Catalysts:  Synthesis and
 Characterization of Novel Dinuclear Nickel(I) Diimine Complexes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              751
_journal_paper_doi               10.1021/om060842s
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C64 H96 Br4 Mg N4 Ni2 O2'
_chemical_formula_weight         1414.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           triclinic
_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                 101.86(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.156(3)
_cell_length_b                   16.357(3)
_cell_length_c                   16.792(3)
_cell_measurement_temperature    220(2)
_cell_volume                     3536.4(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.1421
_diffrn_reflns_av_sigmaI/netI    0.1249
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22424
_diffrn_reflns_theta_full        24.15
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.842
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.755
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.755
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.268
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0684P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                2779
_reflns_number_total             5461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060842ssi20060914_100249.cif
_cod_data_source_block           mei550
_cod_original_cell_volume        3536.1(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4072574
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
C11 C 0.5756(8) 0.6328(7) 0.1773(6) 0.103(3) Uani 1 1 d .
H11A H 0.5040 0.6406 0.1800 0.154 Uiso 1 1 calc R
H11B H 0.5807 0.5914 0.1378 0.154 Uiso 1 1 calc R
H11C H 0.6035 0.6832 0.1618 0.154 Uiso 1 1 calc R
Br2 Br 1.02459(6) 0.66143(4) 0.48857(5) 0.0634(3) Uani 1 1 d .
Ni1 Ni 0.92644(6) 0.65364(5) 0.35050(5) 0.0402(2) Uani 1 1 d .
Br1 Br 0.90227(6) 0.50744(4) 0.34715(4) 0.0534(2) Uani 1 1 d .
Mg2 Mg 1.0000 0.5000 0.5000 0.0469(8) Uani 1 2 d S
C8 C 0.7665(9) 0.9391(6) 0.3957(7) 0.120(4) Uani 1 1 d .
H8A H 0.7274 0.9596 0.4338 0.180 Uiso 1 1 calc R
H8B H 0.7230 0.9375 0.3423 0.180 Uiso 1 1 calc R
H8C H 0.8248 0.9743 0.3952 0.180 Uiso 1 1 calc R
N2 N 0.8088(4) 0.7205(3) 0.3071(3) 0.0422(14) Uani 1 1 d .
N3 N 0.9775(4) 0.7042(3) 0.2644(3) 0.0411(13) Uani 1 1 d .
C16 C 0.9132(5) 0.7537(4) 0.2164(4) 0.0485(18) Uani 1 1 d .
C2 C 0.6395(5) 0.6723(4) 0.3244(5) 0.057(2) Uani 1 1 d .
C17 C 1.0806(5) 0.6909(5) 0.2503(5) 0.0536(19) Uani 1 1 d .
C1 C 0.7196(5) 0.7281(4) 0.3434(4) 0.0474(18) Uani 1 1 d .
C13 C 0.8145(5) 0.7627(4) 0.2401(4) 0.0436(17) Uani 1 1 d .
C6 C 0.7202(6) 0.7893(5) 0.4008(5) 0.060(2) Uani 1 1 d .
C10 C 0.6363(6) 0.6065(5) 0.2597(5) 0.065(2) Uani 1 1 d .
H10 H 0.7081 0.5988 0.2536 0.079 Uiso 1 1 calc R
C26 C 1.0111(7) 0.5690(5) 0.1606(5) 0.064(2) Uani 1 1 d .
H26 H 0.9536 0.5759 0.1889 0.077 Uiso 1 1 calc R
C23 C 1.1455(7) 0.8080(6) 0.3479(6) 0.078(3) Uani 1 1 d .
H23 H 1.0770 0.7999 0.3610 0.094 Uiso 1 1 calc R
C18 C 1.0974(6) 0.6263(5) 0.2003(5) 0.063(2) Uani 1 1 d .
C22 C 1.1605(6) 0.7405(5) 0.2907(5) 0.067(2) Uani 1 1 d .
C15 C 0.9349(6) 0.7985(5) 0.1435(5) 0.066(2) Uani 1 1 d .
H15A H 0.9341 0.8564 0.1530 0.100 Uiso 1 1 calc R
H15B H 0.8826 0.7850 0.0965 0.100 Uiso 1 1 calc R
H15C H 1.0019 0.7828 0.1343 0.100 Uiso 1 1 calc R
C7 C 0.8054(7) 0.8529(6) 0.4207(6) 0.083(3) Uani 1 1 d .
H7 H 0.8577 0.8392 0.3890 0.099 Uiso 1 1 calc R
C14 C 0.7321(6) 0.8185(5) 0.1950(5) 0.070(2) Uani 1 1 d .
H14A H 0.6739 0.8188 0.2213 0.105 Uiso 1 1 calc R
H14B H 0.7101 0.7996 0.1400 0.105 Uiso 1 1 calc R
H14C H 0.7596 0.8729 0.1947 0.105 Uiso 1 1 calc R
C28 C 0.9701(8) 0.5910(6) 0.0716(5) 0.089(3) Uani 1 1 d .
H28A H 0.9480 0.6471 0.0677 0.134 Uiso 1 1 calc R
H28B H 0.9124 0.5563 0.0494 0.134 Uiso 1 1 calc R
H28C H 1.0242 0.5835 0.0416 0.134 Uiso 1 1 calc R
C19 C 1.1980(8) 0.6152(7) 0.1880(6) 0.096(3) Uani 1 1 d .
H19 H 1.2121 0.5728 0.1549 0.115 Uiso 1 1 calc R
C3 C 0.5583(7) 0.6791(6) 0.3650(6) 0.081(3) Uani 1 1 d .
H3 H 0.5027 0.6431 0.3524 0.097 Uiso 1 1 calc R
C27 C 1.0416(9) 0.4786(5) 0.1669(6) 0.104(3) Uani 1 1 d .
H27A H 1.0968 0.4693 0.1384 0.155 Uiso 1 1 calc R
H27B H 0.9827 0.4458 0.1432 0.155 Uiso 1 1 calc R
H27C H 1.0646 0.4641 0.2231 0.155 Uiso 1 1 calc R
C24 C 1.2235(8) 0.8071(7) 0.4268(6) 0.105(4) Uani 1 1 d .
H24A H 1.2277 0.7531 0.4496 0.157 Uiso 1 1 calc R
H24B H 1.2025 0.8449 0.4641 0.157 Uiso 1 1 calc R
H24C H 1.2903 0.8228 0.4173 0.157 Uiso 1 1 calc R
C4 C 0.5578(8) 0.7379(7) 0.4236(7) 0.095(3) Uani 1 1 d .
H4 H 0.5035 0.7409 0.4513 0.114 Uiso 1 1 calc R
C9 C 0.8597(8) 0.8540(7) 0.5090(6) 0.112(4) Uani 1 1 d .
H9A H 0.8132 0.8746 0.5414 0.168 Uiso 1 1 calc R
H9B H 0.9198 0.8887 0.5156 0.168 Uiso 1 1 calc R
H9C H 0.8808 0.7995 0.5262 0.168 Uiso 1 1 calc R
C25 C 1.1447(9) 0.8937(6) 0.3082(7) 0.119(4) Uani 1 1 d .
H25A H 1.2122 0.9053 0.2976 0.178 Uiso 1 1 calc R
H25B H 1.1273 0.9342 0.3445 0.178 Uiso 1 1 calc R
H25C H 1.0942 0.8946 0.2581 0.178 Uiso 1 1 calc R
C5 C 0.6380(8) 0.7916(6) 0.4401(6) 0.082(3) Uani 1 1 d .
H5 H 0.6376 0.8314 0.4796 0.099 Uiso 1 1 calc R
C20 C 1.2768(8) 0.6666(10) 0.2245(8) 0.121(4) Uani 1 1 d .
H20 H 1.3434 0.6595 0.2149 0.146 Uiso 1 1 calc R
C21 C 1.2583(8) 0.7279(8) 0.2746(7) 0.103(4) Uani 1 1 d .
H21 H 1.3126 0.7620 0.2985 0.124 Uiso 1 1 calc R
C32 C 1.3097(17) 0.4978(14) 0.4398(14) 0.239(9) Uiso 1 1 d .
H32A H 1.3306 0.5308 0.3980 0.287 Uiso 1 1 calc R
H32B H 1.3687 0.4911 0.4847 0.287 Uiso 1 1 calc R
C31 C 1.272(2) 0.4237(16) 0.4096(17) 0.289(13) Uiso 1 1 d .
H31A H 1.3197 0.3809 0.4335 0.347 Uiso 1 1 calc R
H31B H 1.2674 0.4228 0.3512 0.347 Uiso 1 1 calc R
C12 C 0.5995(8) 0.5240(6) 0.2830(7) 0.112(4) Uani 1 1 d .
H12A H 0.5279 0.5276 0.2870 0.167 Uiso 1 1 calc R
H12B H 0.6406 0.5075 0.3345 0.167 Uiso 1 1 calc R
H12C H 0.6066 0.4845 0.2422 0.167 Uiso 1 1 calc R
C33 C 1.2219(15) 0.5346(12) 0.4673(12) 0.207(8) Uiso 1 1 d .
H33A H 1.2441 0.5529 0.5232 0.248 Uiso 1 1 calc R
H33B H 1.1980 0.5821 0.4340 0.248 Uiso 1 1 calc R
C30 C 1.1707(15) 0.4077(11) 0.4269(12) 0.210(8) Uiso 1 1 d .
H30A H 1.1211 0.3950 0.3772 0.251 Uiso 1 1 calc R
H30B H 1.1737 0.3621 0.4642 0.251 Uiso 1 1 calc R
O29 O 1.1420(4) 0.4807(3) 0.4626(3) 0.0662(14) Uiso 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'
Ni Ni 0.3393 1.1124 '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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
Ni1 Br2 Mg2 88.17(3) . .
N3 Ni1 N2 81.1(2) . .
N3 Ni1 Br1 118.60(15) . .
N2 Ni1 Br1 117.74(16) . .
N3 Ni1 Br2 120.24(15) . .
N2 Ni1 Br2 124.55(17) . .
Br1 Ni1 Br2 96.70(4) . .
Ni1 Br1 Mg2 89.28(3) . .
O29 Mg2 O29 180.000(1) 3_766 .
O29 Mg2 Br1 90.11(14) 3_766 3_766
O29 Mg2 Br1 89.89(14) . 3_766
O29 Mg2 Br1 89.89(14) 3_766 .
O29 Mg2 Br1 90.11(14) . .
Br1 Mg2 Br1 180.0 3_766 .
O29 Mg2 Br2 90.05(15) 3_766 .
O29 Mg2 Br2 89.95(15) . .
Br1 Mg2 Br2 94.23(2) 3_766 .
Br1 Mg2 Br2 85.77(2) . .
O29 Mg2 Br2 89.95(15) 3_766 3_766
O29 Mg2 Br2 90.05(15) . 3_766
Br1 Mg2 Br2 85.77(2) 3_766 3_766
Br1 Mg2 Br2 94.23(2) . 3_766
Br2 Mg2 Br2 180.0 . 3_766
C13 N2 C1 120.4(5) . .
C13 N2 Ni1 115.8(5) . .
C1 N2 Ni1 123.8(4) . .
C16 N3 C17 120.0(6) . .
C16 N3 Ni1 116.6(5) . .
C17 N3 Ni1 123.4(4) . .
N3 C16 C13 113.3(6) . .
N3 C16 C15 126.2(7) . .
C13 C16 C15 120.5(6) . .
C1 C2 C3 117.5(8) . .
C1 C2 C10 122.7(7) . .
C3 C2 C10 119.8(7) . .
C18 C17 C22 122.6(7) . .
C18 C17 N3 119.0(7) . .
C22 C17 N3 118.3(7) . .
C2 C1 C6 122.1(8) . .
C2 C1 N2 119.8(7) . .
C6 C1 N2 118.0(7) . .
N2 C13 C16 112.9(6) . .
N2 C13 C14 125.5(7) . .
C16 C13 C14 121.4(6) . .
C5 C6 C1 117.3(8) . .
C5 C6 C7 119.6(8) . .
C1 C6 C7 123.1(8) . .
C11 C10 C2 112.6(7) . .
C11 C10 C12 110.7(8) . .
C2 C10 C12 114.2(8) . .
C18 C26 C28 111.5(7) . .
C18 C26 C27 113.9(7) . .
C28 C26 C27 109.4(7) . .
C22 C23 C24 113.7(8) . .
C22 C23 C25 112.4(8) . .
C24 C23 C25 109.3(8) . .
C17 C18 C19 117.4(8) . .
C17 C18 C26 122.5(7) . .
C19 C18 C26 120.1(8) . .
C17 C22 C21 117.2(9) . .
C17 C22 C23 123.8(8) . .
C21 C22 C23 118.9(9) . .
C9 C7 C6 113.9(9) . .
C9 C7 C8 108.9(8) . .
C6 C7 C8 112.4(8) . .
C20 C19 C18 120.3(10) . .
C2 C3 C4 121.7(9) . .
C5 C4 C3 118.7(10) . .
C4 C5 C6 122.6(9) . .
C19 C20 C21 120.7(10) . .
C20 C21 C22 121.4(11) . .
C31 C32 C33 103(2) . .
C32 C31 C30 111(2) . .
O29 C33 C32 111.4(16) . .
O29 C30 C31 105.6(17) . .
C33 O29 C30 107.4(12) . .
C33 O29 Mg2 127.2(9) . .
C30 O29 Mg2 125.4(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C11 C10 1.511(11) .
Br2 Ni1 2.4142(13) .
Br2 Mg2 2.6718(9) .
Ni1 N3 1.904(6) .
Ni1 N2 1.912(5) .
Ni1 Br1 2.4115(11) .
Br1 Mg2 2.6267(10) .
Mg2 O29 2.113(5) 3_766
Mg2 O29 2.113(5) .
Mg2 Br1 2.6267(10) 3_766
Mg2 Br2 2.6719(9) 3_766
C8 C7 1.529(13) .
N2 C13 1.335(8) .
N2 C1 1.435(8) .
N3 C16 1.319(8) .
N3 C17 1.441(8) .
C16 C13 1.440(9) .
C16 C15 1.505(10) .
C2 C1 1.382(10) .
C2 C3 1.385(11) .
C2 C10 1.522(11) .
C17 C18 1.394(10) .
C17 C22 1.389(11) .
C1 C6 1.390(10) .
C13 C14 1.499(9) .
C6 C5 1.377(11) .
C6 C7 1.515(12) .
C10 C12 1.512(11) .
C26 C18 1.517(11) .
C26 C28 1.524(11) .
C26 C27 1.529(11) .
C23 C22 1.502(12) .
C23 C24 1.501(11) .
C23 C25 1.551(12) .
C18 C19 1.393(11) .
C22 C21 1.384(13) .
C7 C9 1.507(12) .
C19 C20 1.377(15) .
C3 C4 1.377(13) .
C4 C5 1.357(13) .
C20 C21 1.362(15) .
C32 C31 1.37(3) .
C32 C33 1.46(2) .
C31 C30 1.44(3) .
C33 O29 1.362(18) .
C30 O29 1.422(18) .
