#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:30:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178716 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/27/4082759.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_4082759
loop_
_publ_author_name
'Minier, Mikael A.'
'Lippard, Stephen J.'
_publ_section_title
;
 Conversion Between Doubly and Triply Carboxylate-Bridged Di(ethylzinc)
 Complexes and Formation of the (μ-Oxo)tetrazinc Carboxylate
 [Zn4O(Ar(Tol)CO2)6].
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1462
_journal_page_last               1466
_journal_paper_doi               10.1021/om5000503
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C54 H60 O6 Zn2'
_chemical_formula_weight         935.76
_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     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.4700(10)
_cell_angle_beta                 97.5130(10)
_cell_angle_gamma                94.7570(10)
_cell_formula_units_Z            1
_cell_length_a                   9.9717(7)
_cell_length_b                   10.6664(8)
_cell_length_c                   11.9804(9)
_cell_measurement_reflns_used    5897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.73
_cell_measurement_theta_min      2.55
_cell_volume                     1136.50(15)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18019
_diffrn_reflns_theta_full        25.79
_diffrn_reflns_theta_max         25.79
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0204P)²+1.0132P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                3585
_reflns_number_total             4343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5000503_si_002.cif
_cod_data_source_block           p-1p
_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/current/ACS/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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4082759--4082761.cif.

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 
;
_cod_original_cell_volume        1136.50(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082759
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
Zn1 Zn 0.34326(3) 0.94207(3) 0.56966(2) 0.01433(8) Uani 1 1 d .
O7A O 0.48079(15) 0.81245(15) 0.53434(14) 0.0156(3) Uani 1 1 d .
O7B O 0.65540(16) 0.96445(15) 0.54441(14) 0.0191(4) Uani 1 1 d .
C1 C 0.7059(2) 0.7634(2) 0.5681(2) 0.0144(5) Uani 1 1 d .
C2 C 0.7019(2) 0.6260(2) 0.4784(2) 0.0153(5) Uani 1 1 d .
C3 C 0.7970(2) 0.5476(2) 0.5019(2) 0.0202(5) Uani 1 1 d .
H3 H 0.7952 0.4544 0.4426 0.024 Uiso 1 1 calc R
C4 C 0.8939(2) 0.6029(2) 0.6097(2) 0.0227(5) Uani 1 1 d .
H4 H 0.9599 0.5487 0.6228 0.027 Uiso 1 1 calc R
C5 C 0.8956(2) 0.7370(2) 0.6992(2) 0.0199(5) Uani 1 1 d .
H5 H 0.9617 0.7738 0.7739 0.024 Uiso 1 1 calc R
C6 C 0.8007(2) 0.8186(2) 0.6803(2) 0.0154(5) Uani 1 1 d .
C7 C 0.6058(2) 0.8531(2) 0.54567(19) 0.0138(5) Uani 1 1 d .
C8 C 0.5999(2) 0.5622(2) 0.3601(2) 0.0159(5) Uani 1 1 d .
C9 C 0.5773(2) 0.6271(2) 0.2809(2) 0.0166(5) Uani 1 1 d .
H9 H 0.6290 0.7152 0.3019 0.020 Uiso 1 1 calc R
C10 C 0.4808(2) 0.5649(2) 0.1722(2) 0.0184(5) Uani 1 1 d .
H10 H 0.4670 0.6113 0.1199 0.022 Uiso 1 1 calc R
C11 C 0.4036(2) 0.4357(2) 0.1381(2) 0.0190(5) Uani 1 1 d .
C12 C 0.4282(2) 0.3700(2) 0.2158(2) 0.0207(5) Uani 1 1 d .
H12 H 0.3778 0.2808 0.1934 0.025 Uiso 1 1 calc R
C13 C 0.5238(2) 0.4306(2) 0.3247(2) 0.0203(5) Uani 1 1 d .
H13 H 0.5383 0.3832 0.3760 0.024 Uiso 1 1 calc R
C14 C 0.2935(2) 0.3704(3) 0.0229(2) 0.0261(6) Uani 1 1 d .
H14A H 0.2772 0.2693 -0.0050 0.039 Uiso 1 1 calc R
H14B H 0.3230 0.3911 -0.0434 0.039 Uiso 1 1 calc R
H14C H 0.2089 0.4085 0.0422 0.039 Uiso 1 1 calc R
C15 C 0.7971(2) 0.9574(2) 0.7851(2) 0.0145(5) Uani 1 1 d .
C16 C 0.6738(2) 0.9970(2) 0.8210(2) 0.0146(5) Uani 1 1 d .
H16 H 0.5904 0.9370 0.7756 0.018 Uiso 1 1 calc R
C17 C 0.6709(2) 1.1220(2) 0.9215(2) 0.0164(5) Uani 1 1 d .
H17 H 0.5854 1.1466 0.9432 0.020 Uiso 1 1 calc R
C18 C 0.7902(2) 1.2121(2) 0.9910(2) 0.0185(5) Uani 1 1 d .
C19 C 0.9133(2) 1.1721(2) 0.9557(2) 0.0200(5) Uani 1 1 d .
H19 H 0.9967 1.2318 1.0020 0.024 Uiso 1 1 calc R
C20 C 0.9173(2) 1.0478(2) 0.8548(2) 0.0193(5) Uani 1 1 d .
H20 H 1.0029 1.0237 0.8328 0.023 Uiso 1 1 calc R
C21 C 0.7869(3) 1.3469(2) 1.1016(2) 0.0243(5) Uani 1 1 d .
H21A H 0.6917 1.3587 1.1096 0.036 Uiso 1 1 calc R
H21B H 0.8316 1.4247 1.0897 0.036 Uiso 1 1 calc R
H21C H 0.8354 1.3451 1.1774 0.036 Uiso 1 1 calc R
O1T O 0.18811(15) 0.78434(15) 0.43807(14) 0.0175(3) Uani 1 1 d .
C2T C 0.2247(2) 0.7048(2) 0.3182(2) 0.0251(6) Uani 1 1 d .
H2T1 H 0.2862 0.6386 0.3240 0.030 Uiso 1 1 calc R
H2T2 H 0.2716 0.7674 0.2886 0.030 Uiso 1 1 calc R
C3T C 0.0906(2) 0.6268(2) 0.2303(2) 0.0214(5) Uani 1 1 d .
H3T1 H 0.0794 0.5273 0.2142 0.026 Uiso 1 1 calc R
H3T2 H 0.0873 0.6330 0.1498 0.026 Uiso 1 1 calc R
C4T C -0.0211(3) 0.6990(2) 0.2981(2) 0.0257(6) Uani 1 1 d .
H4T1 H -0.0826 0.7282 0.2445 0.031 Uiso 1 1 calc R
H4T2 H -0.0762 0.6364 0.3227 0.031 Uiso 1 1 calc R
C5T C 0.0571(2) 0.8241(2) 0.4116(2) 0.0255(6) Uani 1 1 d .
H5T1 H 0.0685 0.9068 0.3939 0.031 Uiso 1 1 calc R
H5T2 H 0.0087 0.8458 0.4830 0.031 Uiso 1 1 calc R
C1E C 0.2984(2) 1.0351(2) 0.7374(2) 0.0210(5) Uani 1 1 d .
H1E1 H 0.3735 1.1119 0.7908 0.025 Uiso 1 1 calc R
H1E2 H 0.2143 1.0767 0.7311 0.025 Uiso 1 1 calc R
C2E C 0.2765(3) 0.9382(3) 0.8003(3) 0.0305(6) Uani 1 1 d .
H2E1 H 0.2550 0.9912 0.8831 0.046 Uiso 1 1 calc R
H2E2 H 0.3600 0.8980 0.8088 0.046 Uiso 1 1 calc R
H2E3 H 0.2005 0.8632 0.7495 0.046 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'
O O 0.0106 0.0060 '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
C1E Zn1 O7A 121.72(8) . .
C1E Zn1 O7B 121.89(8) . 2_676
O7A Zn1 O7B 108.43(6) . 2_676
C1E Zn1 O1T 114.44(8) . .
O7A Zn1 O1T 91.57(6) . .
O7B Zn1 O1T 89.85(6) 2_676 .
C7 O7A Zn1 122.58(13) . .
C7 O7B Zn1 140.55(15) . 2_676
C6 C1 C2 120.81(19) . .
C6 C1 C7 118.98(19) . .
C2 C1 C7 120.2(2) . .
C3 C2 C1 118.4(2) . .
C3 C2 C8 119.2(2) . .
C1 C2 C8 122.42(19) . .
C4 C3 C2 121.2(2) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C3 C4 C5 120.3(2) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
C4 C5 C6 120.5(2) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
C5 C6 C1 118.8(2) . .
C5 C6 C15 118.5(2) . .
C1 C6 C15 122.52(19) . .
O7B C7 O7A 125.6(2) . .
O7B C7 C1 116.96(19) . .
O7A C7 C1 117.36(18) . .
C9 C8 C13 118.0(2) . .
C9 C8 C2 122.62(19) . .
C13 C8 C2 119.4(2) . .
C10 C9 C8 120.9(2) . .
C10 C9 H9 119.6 . .
C8 C9 H9 119.6 . .
C9 C10 C11 121.3(2) . .
C9 C10 H10 119.4 . .
C11 C10 H10 119.4 . .
C12 C11 C10 117.8(2) . .
C12 C11 C14 120.7(2) . .
C10 C11 C14 121.5(2) . .
C13 C12 C11 121.8(2) . .
C13 C12 H12 119.1 . .
C11 C12 H12 119.1 . .
C12 C13 C8 120.3(2) . .
C12 C13 H13 119.8 . .
C8 C13 H13 119.8 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C20 C15 C16 117.6(2) . .
C20 C15 C6 121.1(2) . .
C16 C15 C6 121.1(2) . .
C17 C16 C15 121.2(2) . .
C17 C16 H16 119.4 . .
C15 C16 H16 119.4 . .
C16 C17 C18 121.3(2) . .
C16 C17 H17 119.3 . .
C18 C17 H17 119.3 . .
C17 C18 C19 117.5(2) . .
C17 C18 C21 121.2(2) . .
C19 C18 C21 121.3(2) . .
C20 C19 C18 121.7(2) . .
C20 C19 H19 119.2 . .
C18 C19 H19 119.2 . .
C19 C20 C15 120.7(2) . .
C19 C20 H20 119.6 . .
C15 C20 H20 119.6 . .
C18 C21 H21A 109.5 . .
C18 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C18 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C5T O1T C2T 106.01(17) . .
C5T O1T Zn1 117.45(13) . .
C2T O1T Zn1 115.20(13) . .
O1T C2T C3T 105.71(18) . .
O1T C2T H2T1 110.6 . .
C3T C2T H2T1 110.6 . .
O1T C2T H2T2 110.6 . .
C3T C2T H2T2 110.6 . .
H2T1 C2T H2T2 108.7 . .
C2T C3T C4T 105.06(19) . .
C2T C3T H3T1 110.7 . .
C4T C3T H3T1 110.7 . .
C2T C3T H3T2 110.7 . .
C4T C3T H3T2 110.7 . .
H3T1 C3T H3T2 108.8 . .
C5T C4T C3T 104.23(19) . .
C5T C4T H4T1 110.9 . .
C3T C4T H4T1 110.9 . .
C5T C4T H4T2 110.9 . .
C3T C4T H4T2 110.9 . .
H4T1 C4T H4T2 108.9 . .
O1T C5T C4T 105.03(18) . .
O1T C5T H5T1 110.7 . .
C4T C5T H5T1 110.7 . .
O1T C5T H5T2 110.7 . .
C4T C5T H5T2 110.7 . .
H5T1 C5T H5T2 108.8 . .
C2E C1E Zn1 113.91(16) . .
C2E C1E H1E1 108.8 . .
Zn1 C1E H1E1 108.8 . .
C2E C1E H1E2 108.8 . .
Zn1 C1E H1E2 108.8 . .
H1E1 C1E H1E2 107.7 . .
C1E C2E H2E1 109.5 . .
C1E C2E H2E2 109.5 . .
H2E1 C2E H2E2 109.5 . .
C1E C2E H2E3 109.5 . .
H2E1 C2E H2E3 109.5 . .
H2E2 C2E H2E3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 C1E 1.970(2) .
Zn1 O7A 1.9883(14) .
Zn1 O7B 1.9984(15) 2_676
Zn1 O1T 2.1078(15) .
O7A C7 1.256(3) .
O7B C7 1.255(3) .
O7B Zn1 1.9983(15) 2_676
C1 C6 1.403(3) .
C1 C2 1.407(3) .
C1 C7 1.511(3) .
C2 C3 1.392(3) .
C2 C8 1.489(3) .
C3 C4 1.377(3) .
C3 H3 0.9500 .
C4 C5 1.384(3) .
C4 H4 0.9500 .
C5 C6 1.395(3) .
C5 H5 0.9500 .
C6 C15 1.500(3) .
C8 C9 1.394(3) .
C8 C13 1.404(3) .
C9 C10 1.383(3) .
C9 H9 0.9500 .
C10 C11 1.390(3) .
C10 H10 0.9500 .
C11 C12 1.389(3) .
C11 C14 1.509(3) .
C12 C13 1.380(3) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C20 1.394(3) .
C15 C16 1.396(3) .
C16 C17 1.384(3) .
C16 H16 0.9500 .
C17 C18 1.386(3) .
C17 H17 0.9500 .
C18 C19 1.394(3) .
C18 C21 1.505(3) .
C19 C20 1.384(3) .
C19 H19 0.9500 .
C20 H20 0.9500 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
O1T C5T 1.443(3) .
O1T C2T 1.447(3) .
C2T C3T 1.520(3) .
C2T H2T1 0.9900 .
C2T H2T2 0.9900 .
C3T C4T 1.535(3) .
C3T H3T1 0.9900 .
C3T H3T2 0.9900 .
C4T C5T 1.511(3) .
C4T H4T1 0.9900 .
C4T H4T2 0.9900 .
C5T H5T1 0.9900 .
C5T H5T2 0.9900 .
C1E C2E 1.528(3) .
C1E H1E1 0.9900 .
C1E H1E2 0.9900 .
C2E H2E1 0.9800 .
C2E H2E2 0.9800 .
C2E H2E3 0.9800 .
