#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:12:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178553 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/61/4066177.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_4066177
loop_
_publ_author_name
'Kahnes, Marcel'
'Görls, Helmar'
'Westerhausen, Matthias'
_publ_section_title
;
 Synthesis of Dinuclear Zinc Alkynyls and Their Use in Catalytic
 Silicon−Carbon Bond Formation
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3490
_journal_paper_doi               10.1021/om100338s
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C40 H34 N6 Zn2'
_chemical_formula_sum            'C40 H34 N6 Zn2'
_chemical_formula_weight         729.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   9.9024(2)
_cell_length_b                   14.0656(4)
_cell_length_c                   24.2369(6)
_cell_measurement_reflns_used    19563
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     3375.79(14)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            19563
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0355
_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)+(0.0406P)²+0.6522P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                2811
_reflns_number_total             3865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100338s_si_002.cif
_cod_data_source_block           FO3951
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'NONE' changed to 'none'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthrhombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4066177
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
Zn1 Zn -0.02989(2) 0.071047(17) 0.041913(10) 0.01552(9) Uani 1 1 d
N1 N -0.15931(17) 0.14682(12) -0.01787(7) 0.0178(4) Uani 1 1 d
N2 N 0.08749(18) 0.07009(12) -0.02992(7) 0.0168(4) Uani 1 1 d
N3 N 0.17769(18) 0.06165(12) 0.07520(8) 0.0190(4) Uani 1 1 d
C1 C -0.2886(2) 0.17176(15) -0.00893(11) 0.0213(5) Uani 1 1 d
H1 H -0.315(2) 0.1670(17) 0.0270(10) 0.022(6) Uiso 1 1 d
C2 C -0.3725(3) 0.20335(17) -0.05018(11) 0.0282(6) Uani 1 1 d
H2 H -0.460(3) 0.222(2) -0.0431(10) 0.031(7) Uiso 1 1 d
C3 C -0.3206(3) 0.21036(17) -0.10278(11) 0.0304(6) Uani 1 1 d
H3 H -0.375(2) 0.2326(16) -0.1313(10) 0.024(6) Uiso 1 1 d
C4 C -0.1881(3) 0.18549(17) -0.11252(11) 0.0264(6) Uani 1 1 d
H4 H -0.154(2) 0.1876(16) -0.1460(10) 0.017(6) Uiso 1 1 d
C5 C -0.1088(2) 0.15338(15) -0.06881(9) 0.0185(5) Uani 1 1 d
C6 C 0.0381(2) 0.12742(18) -0.07599(10) 0.0217(5) Uani 1 1 d
H6A H 0.041(2) 0.0950(17) -0.1111(10) 0.020(6) Uiso 1 1 d
H6B H 0.090(2) 0.1896(18) -0.0781(10) 0.031(7) Uiso 1 1 d
C7 C 0.2325(2) 0.07975(18) -0.02257(9) 0.0194(5) Uani 1 1 d
H7B H 0.281(2) 0.0332(18) -0.0426(9) 0.021(6) Uiso 1 1 d
H7A H 0.264(2) 0.1456(18) -0.0351(9) 0.018(6) Uiso 1 1 d
C8 C 0.2750(2) 0.07041(15) 0.03723(9) 0.0195(5) Uani 1 1 d
C9 C 0.4108(2) 0.07442(17) 0.05251(10) 0.0257(6) Uani 1 1 d
H9 H 0.475(2) 0.0823(17) 0.0227(11) 0.025(7) Uiso 1 1 d
C10 C 0.4452(3) 0.07231(18) 0.10745(12) 0.0307(6) Uani 1 1 d
H10 H 0.538(3) 0.0797(18) 0.1173(12) 0.039(8) Uiso 1 1 d
C11 C 0.3444(3) 0.06506(17) 0.14661(11) 0.0283(6) Uani 1 1 d
H11 H 0.366(2) 0.0658(17) 0.1847(11) 0.032(7) Uiso 1 1 d
C12 C 0.2124(2) 0.05943(16) 0.12893(10) 0.0242(5) Uani 1 1 d
H12 H 0.142(2) 0.0545(15) 0.1549(10) 0.020(6) Uiso 1 1 d
C13 C -0.1187(2) 0.13011(17) 0.10796(9) 0.0215(5) Uani 1 1 d
C14 C -0.1803(2) 0.17621(17) 0.14174(9) 0.0217(5) Uani 1 1 d
C15 C -0.2541(2) 0.23534(17) 0.18012(9) 0.0218(5) Uani 1 1 d
C16 C -0.2343(2) 0.33357(19) 0.18094(10) 0.0275(6) Uani 1 1 d
H16 H -0.167(2) 0.3598(17) 0.1554(10) 0.028(7) Uiso 1 1 d
C17 C -0.3085(3) 0.3912(2) 0.21638(12) 0.0360(7) Uani 1 1 d
H17 H -0.297(3) 0.455(2) 0.2163(11) 0.036(8) Uiso 1 1 d
C18 C -0.4031(3) 0.3518(2) 0.25109(12) 0.0422(8) Uani 1 1 d
H18 H -0.451(3) 0.391(2) 0.2764(13) 0.052(9) Uiso 1 1 d
C19 C -0.4234(3) 0.2547(2) 0.25114(12) 0.0403(7) Uani 1 1 d
H19 H -0.485(3) 0.2259(19) 0.2738(12) 0.038(8) Uiso 1 1 d
C20 C -0.3489(2) 0.1967(2) 0.21609(10) 0.0307(6) Uani 1 1 d
H20 H -0.362(2) 0.1306(19) 0.2162(10) 0.030(7) 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'
Zn Zn 0.2839 1.4301 '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
C13 Zn1 N2 112.67(8) . 5
C13 Zn1 N2 155.44(8) . .
N2 Zn1 N2 91.71(7) 5 .
C13 Zn1 N1 93.97(8) . .
N2 Zn1 N1 102.07(7) 5 .
N2 Zn1 N1 77.27(7) . .
C13 Zn1 N3 98.10(8) . .
N2 Zn1 N3 104.36(7) 5 .
N2 Zn1 N3 77.70(7) . .
N1 Zn1 N3 143.83(7) . .
C13 Zn1 Zn1 158.48(7) . 5
N2 Zn1 Zn1 45.96(5) 5 5
N2 Zn1 Zn1 45.75(5) . 5
N1 Zn1 Zn1 89.51(5) . 5
N3 Zn1 Zn1 91.41(5) . 5
C5 N1 C1 119.2(2) . .
C5 N1 Zn1 115.00(14) . .
C1 N1 Zn1 124.93(16) . .
C7 N2 C6 111.89(17) . .
C7 N2 Zn1 112.11(14) . 5
C6 N2 Zn1 109.09(14) . 5
C7 N2 Zn1 116.50(13) . .
C6 N2 Zn1 116.47(14) . .
Zn1 N2 Zn1 88.29(7) 5 .
C8 N3 C12 118.9(2) . .
C8 N3 Zn1 114.37(15) . .
C12 N3 Zn1 126.23(15) . .
N1 C1 C2 122.9(2) . .
N1 C1 H1 114.0(15) . .
C2 C1 H1 123.1(15) . .
C1 C2 C3 118.1(2) . .
C1 C2 H2 121.6(16) . .
C3 C2 H2 120.3(16) . .
C4 C3 C2 119.7(2) . .
C4 C3 H3 120.8(14) . .
C2 C3 H3 119.6(14) . .
C3 C4 C5 119.2(2) . .
C3 C4 H4 120.9(14) . .
C5 C4 H4 119.8(14) . .
N1 C5 C4 120.9(2) . .
N1 C5 C6 116.78(19) . .
C4 C5 C6 122.2(2) . .
N2 C6 C5 111.60(18) . .
N2 C6 H6A 113.7(14) . .
C5 C6 H6A 104.1(13) . .
N2 C6 H6B 110.0(13) . .
C5 C6 H6B 106.8(13) . .
H6A C6 H6B 110.3(19) . .
N2 C7 C8 112.54(18) . .
N2 C7 H7B 111.9(14) . .
C8 C7 H7B 106.9(14) . .
N2 C7 H7A 110.6(12) . .
C8 C7 H7A 106.1(12) . .
H7B C7 H7A 108.6(19) . .
N3 C8 C9 121.0(2) . .
N3 C8 C7 117.8(2) . .
C9 C8 C7 121.2(2) . .
C10 C9 C8 119.7(2) . .
C10 C9 H9 124.0(15) . .
C8 C9 H9 116.3(15) . .
C9 C10 C11 119.2(2) . .
C9 C10 H10 118.5(17) . .
C11 C10 H10 122.2(17) . .
C12 C11 C10 118.4(2) . .
C12 C11 H11 121.0(15) . .
C10 C11 H11 120.5(15) . .
N3 C12 C11 122.8(2) . .
N3 C12 H12 117.4(14) . .
C11 C12 H12 119.8(14) . .
C14 C13 Zn1 169.4(2) . .
C13 C14 C15 177.1(3) . .
C20 C15 C16 118.2(2) . .
C20 C15 C14 121.3(2) . .
C16 C15 C14 120.5(2) . .
C17 C16 C15 120.7(3) . .
C17 C16 H16 122.0(15) . .
C15 C16 H16 117.3(14) . .
C18 C17 C16 120.2(3) . .
C18 C17 H17 119.2(17) . .
C16 C17 H17 120.6(17) . .
C17 C18 C19 119.9(3) . .
C17 C18 H18 119.9(19) . .
C19 C18 H18 120.2(19) . .
C18 C19 C20 120.2(3) . .
C18 C19 H19 122.4(18) . .
C20 C19 H19 117.3(18) . .
C19 C20 C15 120.8(3) . .
C19 C20 H20 120.4(16) . .
C15 C20 H20 118.8(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 C13 2.007(2) .
Zn1 N2 2.0858(18) 5
Zn1 N2 2.0934(17) .
Zn1 N1 2.2085(18) .
Zn1 N3 2.2122(18) .
Zn1 Zn1 2.9108(5) 5
N1 C5 1.335(3) .
N1 C1 1.345(3) .
N2 C7 1.453(3) .
N2 C6 1.462(3) .
N2 Zn1 2.0858(18) 5
N3 C8 1.338(3) .
N3 C12 1.347(3) .
C1 C2 1.374(3) .
C1 H1 0.91(2) .
C2 C3 1.378(4) .
C2 H2 0.92(3) .
C3 C4 1.379(4) .
C3 H3 0.93(2) .
C4 C5 1.394(3) .
C4 H4 0.88(2) .
C5 C6 1.509(3) .
C6 H6A 0.97(2) .
C6 H6B 1.02(2) .
C7 C8 1.515(3) .
C7 H7B 0.94(2) .
C7 H7A 1.02(2) .
C8 C9 1.396(3) .
C9 C10 1.375(4) .
C9 H9 0.97(3) .
C10 C11 1.381(4) .
C10 H10 0.96(3) .
C11 C12 1.378(3) .
C11 H11 0.95(3) .
C12 H12 0.94(2) .
C13 C14 1.210(3) .
C14 C15 1.446(3) .
C15 C20 1.392(3) .
C15 C16 1.396(3) .
C16 C17 1.391(3) .
C16 H16 0.98(2) .
C17 C18 1.376(4) .
C17 H17 0.90(3) .
C18 C19 1.380(4) .
C18 H18 0.95(3) .
C19 C20 1.389(4) .
C19 H19 0.91(3) .
C20 H20 0.94(3) .
