#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:28:59 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179972 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/66/7026679.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_7026679
loop_
_publ_author_name
'Jones, Cameron'
'Furness, Leigh'
'Nembenna, Sharanappa'
'Rose, Richard P.'
'Aldridge, Simon'
'Stasch, Andreas'
_publ_section_title
;
 Bulky guanidinato and amidinato zinc complexes and their comparative
 stabilities.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8788
_journal_page_last               8795
_journal_paper_doi               10.1039/c0dt00589d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C58 H86 Br2 N4 Zn2'
_chemical_formula_weight         1129.87
_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                105.869(2)
_cell_angle_beta                 102.254(2)
_cell_angle_gamma                106.999(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0698(3)
_cell_length_b                   10.7948(4)
_cell_length_c                   14.8844(7)
_cell_measurement_temperature    123(2)
_cell_volume                     1411.22(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21361
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    2.304
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0399
_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)+(0.0307P)²+0.3004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                3983
_reflns_number_total             6293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00589d.txt
_cod_data_source_block           compound5
_cod_original_cell_volume        1411.22(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7026679
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
Br1 Br 0.32046(3) 0.94551(4) 0.016905(19) 0.02397(10) Uani 1 1 d .
Zn1 Zn 0.57724(4) 1.02075(4) 0.11156(2) 0.01902(11) Uani 1 1 d .
N1 N 0.6615(2) 1.1408(3) 0.25395(15) 0.0160(6) Uani 1 1 d .
C1 C 0.6843(3) 1.0373(3) 0.28007(19) 0.0146(7) Uani 1 1 d .
N2 N 0.6402(2) 0.9229(3) 0.19918(16) 0.0168(6) Uani 1 1 d .
C2 C 0.7502(3) 1.0499(3) 0.38660(19) 0.0197(7) Uani 1 1 d .
C3 C 0.7599(3) 0.9152(3) 0.3965(2) 0.0233(8) Uani 1 1 d .
H3A H 0.6618 0.8423 0.3690 0.035 Uiso 1 1 calc R
H3B H 0.8005 0.9302 0.4662 0.035 Uiso 1 1 calc R
H3C H 0.8235 0.8869 0.3605 0.035 Uiso 1 1 calc R
C4 C 0.6540(4) 1.0929(4) 0.4474(2) 0.0315(9) Uani 1 1 d .
H4A H 0.6561 1.1851 0.4497 0.047 Uiso 1 1 calc R
H4B H 0.6917 1.0955 0.5145 0.047 Uiso 1 1 calc R
H4C H 0.5530 1.0255 0.4167 0.047 Uiso 1 1 calc R
C5 C 0.9046(3) 1.1611(4) 0.4310(2) 0.0303(9) Uani 1 1 d .
H5A H 0.9636 1.1394 0.3889 0.046 Uiso 1 1 calc R
H5B H 0.9497 1.1634 0.4969 0.046 Uiso 1 1 calc R
H5C H 0.8995 1.2518 0.4356 0.046 Uiso 1 1 calc R
C6 C 0.6909(3) 1.2819(3) 0.30874(18) 0.0155(7) Uani 1 1 d .
C7 C 0.5772(3) 1.3187(3) 0.33652(19) 0.0181(7) Uani 1 1 d .
C8 C 0.6024(3) 1.4586(3) 0.3796(2) 0.0222(7) Uani 1 1 d .
H8 H 0.5279 1.4839 0.4002 0.027 Uiso 1 1 calc R
C9 C 0.7317(3) 1.5612(4) 0.3933(2) 0.0238(8) Uani 1 1 d .
H9 H 0.7463 1.6561 0.4229 0.029 Uiso 1 1 calc R
C10 C 0.8409(3) 1.5244(3) 0.3632(2) 0.0213(7) Uani 1 1 d .
H10 H 0.9298 1.5953 0.3716 0.026 Uiso 1 1 calc R
C11 C 0.8230(3) 1.3870(3) 0.32145(19) 0.0178(7) Uani 1 1 d .
C12 C 0.4259(3) 1.2116(4) 0.3122(2) 0.0217(7) Uani 1 1 d .
H12 H 0.4305 1.1172 0.2894 0.026 Uiso 1 1 calc R
C13 C 0.3194(3) 1.2240(4) 0.2275(2) 0.0295(8) Uani 1 1 d .
H13A H 0.3100 1.3144 0.2495 0.044 Uiso 1 1 calc R
H13B H 0.2232 1.1499 0.2075 0.044 Uiso 1 1 calc R
H13C H 0.3569 1.2157 0.1714 0.044 Uiso 1 1 calc R
C14 C 0.3684(3) 1.2265(4) 0.4014(2) 0.0311(9) Uani 1 1 d .
H14A H 0.4388 1.2227 0.4562 0.047 Uiso 1 1 calc R
H14B H 0.2740 1.1507 0.3830 0.047 Uiso 1 1 calc R
H14C H 0.3560 1.3157 0.4215 0.047 Uiso 1 1 calc R
C15 C 0.9440(3) 1.3541(4) 0.2850(2) 0.0220(7) Uani 1 1 d .
H15 H 0.9233 1.2528 0.2694 0.026 Uiso 1 1 calc R
C16 C 0.9448(3) 1.3857(4) 0.1903(2) 0.0270(8) Uani 1 1 d .
H16A H 0.8464 1.3379 0.1421 0.041 Uiso 1 1 calc R
H16B H 1.0140 1.3532 0.1630 0.041 Uiso 1 1 calc R
H16C H 0.9744 1.4859 0.2057 0.041 Uiso 1 1 calc R
C17 C 1.0955(3) 1.4358(4) 0.3627(2) 0.0307(9) Uani 1 1 d .
H17A H 1.1200 1.5353 0.3763 0.046 Uiso 1 1 calc R
H17B H 1.1688 1.4073 0.3381 0.046 Uiso 1 1 calc R
H17C H 1.0945 1.4171 0.4235 0.046 Uiso 1 1 calc R
C18 C 0.6332(3) 0.7857(3) 0.18339(18) 0.0175(7) Uani 1 1 d .
C19 C 0.5031(3) 0.6821(4) 0.1742(2) 0.0207(7) Uani 1 1 d .
C20 C 0.4945(3) 0.5464(4) 0.1490(2) 0.0273(8) Uani 1 1 d .
H20 H 0.4075 0.4764 0.1445 0.033 Uiso 1 1 calc R
C21 C 0.6089(4) 0.5098(4) 0.1302(2) 0.0275(8) Uani 1 1 d .
H21 H 0.6011 0.4159 0.1128 0.033 Uiso 1 1 calc R
C22 C 0.7341(3) 0.6115(4) 0.1371(2) 0.0266(8) Uani 1 1 d .
H22 H 0.8123 0.5860 0.1233 0.032 Uiso 1 1 calc R
C23 C 0.7507(3) 0.7491(4) 0.1631(2) 0.0225(8) Uani 1 1 d .
C24 C 0.3710(3) 0.7166(4) 0.1902(2) 0.0246(8) Uani 1 1 d .
H24 H 0.3949 0.8178 0.2032 0.030 Uiso 1 1 calc R
C25 C 0.2365(3) 0.6342(4) 0.0976(2) 0.0329(9) Uani 1 1 d .
H25A H 0.2610 0.6508 0.0406 0.049 Uiso 1 1 calc R
H25B H 0.1558 0.6643 0.1066 0.049 Uiso 1 1 calc R
H25C H 0.2070 0.5350 0.0867 0.049 Uiso 1 1 calc R
C26 C 0.3357(3) 0.6858(4) 0.2790(2) 0.0353(9) Uani 1 1 d .
H26A H 0.3110 0.5867 0.2671 0.053 Uiso 1 1 calc R
H26B H 0.2524 0.7110 0.2885 0.053 Uiso 1 1 calc R
H26C H 0.4211 0.7401 0.3382 0.053 Uiso 1 1 calc R
C27 C 0.8903(3) 0.8568(4) 0.1664(2) 0.0277(8) Uani 1 1 d .
H27 H 0.8844 0.9503 0.1912 0.033 Uiso 1 1 calc R
C28 C 0.9049(4) 0.8315(4) 0.0625(2) 0.0399(10) Uani 1 1 d .
H28A H 0.9918 0.9054 0.0655 0.060 Uiso 1 1 calc R
H28B H 0.8176 0.8313 0.0182 0.060 Uiso 1 1 calc R
H28C H 0.9145 0.7416 0.0378 0.060 Uiso 1 1 calc R
C29 C 1.0265(3) 0.8574(4) 0.2365(2) 0.0407(10) Uani 1 1 d .
H29A H 1.0195 0.8797 0.3033 0.061 Uiso 1 1 calc R
H29B H 1.1142 0.9272 0.2364 0.061 Uiso 1 1 calc R
H29C H 1.0329 0.7657 0.2146 0.061 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'
Zn Zn 0.2839 1.4301 '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
Zn1 Br1 Zn1 82.476(14) 2_675 .
N1 Zn1 N2 66.64(10) . .
N1 Zn1 Br1 126.04(7) . 2_675
N2 Zn1 Br1 123.67(7) . 2_675
N1 Zn1 Br1 123.26(7) . .
N2 Zn1 Br1 120.54(7) . .
Br1 Zn1 Br1 97.524(14) 2_675 .
N1 Zn1 C1 33.28(10) . .
N2 Zn1 C1 33.36(10) . .
Br1 Zn1 C1 133.30(6) 2_675 .
Br1 Zn1 C1 129.05(6) . .
C1 N1 C6 132.8(2) . .
C1 N1 Zn1 92.08(18) . .
C6 N1 Zn1 135.07(19) . .
N1 C1 N2 109.6(2) . .
N1 C1 C2 124.3(3) . .
N2 C1 C2 126.1(3) . .
N1 C1 Zn1 54.64(13) . .
N2 C1 Zn1 54.94(14) . .
C2 C1 Zn1 178.8(2) . .
C1 N2 C18 133.9(2) . .
C1 N2 Zn1 91.70(19) . .
C18 N2 Zn1 134.33(17) . .
C5 C2 C3 107.9(3) . .
C5 C2 C1 109.6(2) . .
C3 C2 C1 113.9(2) . .
C5 C2 C4 109.0(3) . .
C3 C2 C4 107.5(2) . .
C1 C2 C4 108.9(2) . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C2 C5 H5A 109.5 . .
C2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C11 C6 C7 119.6(3) . .
C11 C6 N1 120.3(3) . .
C7 C6 N1 119.3(3) . .
C8 C7 C6 118.6(3) . .
C8 C7 C12 119.1(3) . .
C6 C7 C12 122.0(3) . .
C9 C8 C7 121.9(3) . .
C9 C8 H8 119.0 . .
C7 C8 H8 119.0 . .
C8 C9 C10 119.1(3) . .
C8 C9 H9 120.4 . .
C10 C9 H9 120.4 . .
C11 C10 C9 121.5(3) . .
C11 C10 H10 119.3 . .
C9 C10 H10 119.3 . .
C10 C11 C6 119.2(3) . .
C10 C11 C15 118.7(3) . .
C6 C11 C15 122.0(3) . .
C7 C12 C13 109.0(3) . .
C7 C12 C14 112.9(2) . .
C13 C12 C14 109.8(2) . .
C7 C12 H12 108.4 . .
C13 C12 H12 108.4 . .
C14 C12 H12 108.4 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C11 C15 C17 112.1(2) . .
C11 C15 C16 110.2(3) . .
C17 C15 C16 109.4(2) . .
C11 C15 H15 108.3 . .
C17 C15 H15 108.3 . .
C16 C15 H15 108.3 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C19 C18 N2 120.2(3) . .
C19 C18 C23 119.8(3) . .
N2 C18 C23 119.5(3) . .
C20 C19 C18 119.0(3) . .
C20 C19 C24 119.8(3) . .
C18 C19 C24 121.3(3) . .
C19 C20 C21 121.7(3) . .
C19 C20 H20 119.1 . .
C21 C20 H20 119.1 . .
C22 C21 C20 118.8(3) . .
C22 C21 H21 120.6 . .
C20 C21 H21 120.6 . .
C21 C22 C23 122.5(3) . .
C21 C22 H22 118.7 . .
C23 C22 H22 118.7 . .
C22 C23 C18 118.2(3) . .
C22 C23 C27 120.2(3) . .
C18 C23 C27 121.5(3) . .
C19 C24 C26 111.2(3) . .
C19 C24 C25 110.5(3) . .
C26 C24 C25 109.8(3) . .
C19 C24 H24 108.4 . .
C26 C24 H24 108.4 . .
C25 C24 H24 108.4 . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 C26 H26A 109.5 . .
C24 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C24 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C23 C27 C29 111.7(3) . .
C23 C27 C28 110.7(3) . .
C29 C27 C28 109.9(3) . .
C23 C27 H27 108.1 . .
C29 C27 H27 108.1 . .
C28 C27 H27 108.1 . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Zn1 2.4182(4) 2_675
Br1 Zn1 2.4352(4) .
Zn1 N1 1.996(2) .
Zn1 N2 2.003(2) .
Zn1 Br1 2.4182(4) 2_675
Zn1 C1 2.446(3) .
N1 C1 1.343(4) .
N1 C6 1.424(4) .
C1 N2 1.345(4) .
C1 C2 1.535(4) .
N2 C18 1.412(4) .
C2 C5 1.528(4) .
C2 C3 1.529(4) .
C2 C4 1.542(4) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C11 1.409(4) .
C6 C7 1.420(4) .
C7 C8 1.390(4) .
C7 C12 1.516(4) .
C8 C9 1.373(4) .
C8 H8 0.9500 .
C9 C10 1.392(4) .
C9 H9 0.9500 .
C10 C11 1.382(4) .
C10 H10 0.9500 .
C11 C15 1.527(4) .
C12 C13 1.536(4) .
C12 C14 1.545(4) .
C12 H12 1.0000 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C17 1.533(4) .
C15 C16 1.539(4) .
C15 H15 1.0000 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 C19 1.404(4) .
C18 C23 1.417(4) .
C19 C20 1.380(4) .
C19 C24 1.530(4) .
C20 C21 1.380(4) .
C20 H20 0.9500 .
C21 C22 1.371(4) .
C21 H21 0.9500 .
C22 C23 1.377(5) .
C22 H22 0.9500 .
C23 C27 1.521(4) .
C24 C26 1.534(4) .
C24 C25 1.535(4) .
C24 H24 1.0000 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 C29 1.534(4) .
C27 C28 1.541(4) .
C27 H27 1.0000 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
