#------------------------------------------------------------------------------
#$Date: 2018-09-01 02:01:52 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/83/4308385.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_4308385
loop_
_publ_author_name
'Tang, Yongjun'
'Kassel, W. Scott'
'Zakharov, Lev N.'
'Rheingold, Arnold L.'
'Kemp, Richard A.'
_publ_section_title
;
 Insertion Reactions of Carbon Dioxide into Zn--N Bonds: Syntheses and
 Structures of Tetrameric and Dimeric Alkylzinc Carbamato Complexes
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              359
_journal_page_last               364
_journal_paper_doi               10.1021/ic048830r
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C30 H52 N4 O4 Zn2'
_chemical_formula_weight         663.50
_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                93.746(2)
_cell_angle_beta                 114.231(2)
_cell_angle_gamma                95.017(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2058(10)
_cell_length_b                   9.4827(10)
_cell_length_c                   10.5975(11)
_cell_measurement_reflns_used    4757
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.48
_cell_volume                     835.15(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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5270
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0508P)²+0.3295P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                3550
_reflns_number_total             3684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048830rsi20041020_055906_5.cif
_cod_data_source_block           Compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4308385
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.014367(19) -0.087533(17) 0.830398(17) 0.01808(8) Uani 1 1 d . . .
N1 N 0.23133(16) -0.11641(14) 0.81219(14) 0.0213(3) Uani 1 1 d . . .
N2 N -0.03153(16) 0.29631(14) 0.83669(13) 0.0185(2) Uani 1 1 d . . .
O1 O 0.05775(14) -0.21725(12) 0.97642(12) 0.0222(2) Uani 1 1 d . . .
O2 O 0.09592(13) 0.11035(11) 0.93838(12) 0.0201(2) Uani 1 1 d . . .
C1 C -0.1718(2) -0.09067(19) 0.64852(17) 0.0253(3) Uani 1 1 d . . .
H1B H -0.2679 -0.0768 0.6639 0.038 Uiso 1 1 calc R . .
H1C H -0.1893 -0.1827 0.5934 0.038 Uiso 1 1 calc R . .
H1D H -0.1505 -0.0140 0.5984 0.038 Uiso 1 1 calc R . .
C2 C 0.00333(17) 0.20385(15) 0.93562(15) 0.0176(3) Uani 1 1 d . . .
C3 C 0.02668(19) 0.28498(17) 0.72756(16) 0.0218(3) Uani 1 1 d . . .
H3A H -0.0669 0.2634 0.6362 0.026 Uiso 1 1 calc R . .
H3B H 0.0905 0.2040 0.7410 0.026 Uiso 1 1 calc R . .
C4 C 0.1295(2) 0.41869(18) 0.72418(19) 0.0259(3) Uani 1 1 d . . .
H4A H 0.0664 0.5011 0.7146 0.031 Uiso 1 1 calc R . .
C5 C 0.2830(2) 0.4504(2) 0.8576(2) 0.0360(4) Uani 1 1 d . . .
H5A H 0.2557 0.4626 0.9375 0.054 Uiso 1 1 calc R . .
H5B H 0.3451 0.5380 0.8535 0.054 Uiso 1 1 calc R . .
H5C H 0.3470 0.3711 0.8676 0.054 Uiso 1 1 calc R . .
C6 C 0.1677(3) 0.3990(2) 0.5974(2) 0.0378(4) Uani 1 1 d . . .
H6A H 0.0673 0.3788 0.5128 0.057 Uiso 1 1 calc R . .
H6B H 0.2309 0.3194 0.6060 0.057 Uiso 1 1 calc R . .
H6C H 0.2292 0.4863 0.5919 0.057 Uiso 1 1 calc R . .
C7 C -0.12963(18) 0.41041(16) 0.83532(16) 0.0193(3) Uani 1 1 d . . .
H7A H -0.0643 0.5032 0.8478 0.023 Uiso 1 1 calc R . .
H7B H -0.1579 0.4070 0.9158 0.023 Uiso 1 1 calc R . .
C8 C -0.2842(2) 0.40313(18) 0.70267(17) 0.0242(3) Uani 1 1 d . . .
H8A H -0.2554 0.4066 0.6215 0.029 Uiso 1 1 calc R . .
C9 C -0.3947(2) 0.2660(2) 0.6805(2) 0.0378(5) Uani 1 1 d . . .
H9A H -0.3391 0.1842 0.6743 0.057 Uiso 1 1 calc R . .
H9B H -0.4916 0.2641 0.5939 0.057 Uiso 1 1 calc R . .
H9C H -0.4247 0.2615 0.7589 0.057 Uiso 1 1 calc R . .
C10 C -0.3663(2) 0.5342(2) 0.7128(2) 0.0317(4) Uani 1 1 d . . .
H10A H -0.4658 0.5316 0.6284 0.048 Uiso 1 1 calc R . .
H10B H -0.2944 0.6206 0.7222 0.048 Uiso 1 1 calc R . .
H10C H -0.3913 0.5342 0.7942 0.048 Uiso 1 1 calc R . .
C11 C 0.2512(2) -0.0802(2) 0.70003(19) 0.0307(4) Uani 1 1 d . . .
H11A H 0.1623 -0.0522 0.6251 0.037 Uiso 1 1 calc R . .
C12 C 0.3956(3) -0.0816(2) 0.6880(2) 0.0378(4) Uani 1 1 d . . .
H12A H 0.4055 -0.0546 0.6069 0.045 Uiso 1 1 calc R . .
C13 C 0.5247(2) -0.1230(2) 0.7968(2) 0.0338(4) Uani 1 1 d . . .
H13A H 0.6252 -0.1248 0.7918 0.041 Uiso 1 1 calc R . .
C14 C 0.5053(2) -0.1614(2) 0.9123(2) 0.0333(4) Uani 1 1 d . . .
H14A H 0.5922 -0.1904 0.9883 0.040 Uiso 1 1 calc R . .
C15 C 0.3568(2) -0.15724(19) 0.91609(19) 0.0276(3) Uani 1 1 d . . .
H15A H 0.3438 -0.1845 0.9959 0.033 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'
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
_geom_angle_publ_flag
O1 Zn1 C1 130.92(6) . . ?
O1 Zn1 O2 104.15(5) . . ?
C1 Zn1 O2 113.74(6) . . ?
O1 Zn1 N1 92.25(5) . . ?
C1 Zn1 N1 113.39(6) . . ?
O2 Zn1 N1 95.02(5) . . ?
C11 N1 C15 117.82(14) . . ?
C11 N1 Zn1 119.95(11) . . ?
C15 N1 Zn1 121.91(11) . . ?
C2 N2 C3 121.37(13) . . ?
C2 N2 C7 121.23(12) . . ?
C3 N2 C7 117.40(12) . . ?
C2 O1 Zn1 120.10(10) 2_557 . ?
C2 O2 Zn1 123.01(9) . . ?
O2 C2 O1 122.85(14) . 2_557 ?
O2 C2 N2 119.71(13) . . ?
O1 C2 N2 117.43(13) 2_557 . ?
N2 C3 C4 114.20(13) . . ?
C5 C4 C6 110.86(15) . . ?
C5 C4 C3 111.26(14) . . ?
C6 C4 C3 109.01(15) . . ?
N2 C7 C8 114.52(13) . . ?
C9 C8 C7 111.61(14) . . ?
C9 C8 C10 111.33(15) . . ?
C7 C8 C10 108.21(14) . . ?
N1 C11 C12 122.99(18) . . ?
C13 C12 C11 118.53(18) . . ?
C14 C13 C12 118.96(17) . . ?
C13 C14 C15 118.96(18) . . ?
N1 C15 C14 122.74(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.9735(11) . ?
Zn1 C1 1.9814(17) . ?
Zn1 O2 2.0401(11) . ?
Zn1 N1 2.1229(13) . ?
N1 C11 1.336(2) . ?
N1 C15 1.337(2) . ?
N2 C2 1.365(2) . ?
N2 C3 1.4624(19) . ?
N2 C7 1.4658(19) . ?
O1 C2 1.2761(19) 2_557 ?
O2 C2 1.2762(18) . ?
C2 O1 1.2761(19) 2_557 ?
C3 C4 1.526(2) . ?
C4 C5 1.522(3) . ?
C4 C6 1.526(2) . ?
C7 C8 1.528(2) . ?
C8 C9 1.521(3) . ?
C8 C10 1.530(2) . ?
C11 C12 1.388(3) . ?
C12 C13 1.383(3) . ?
C13 C14 1.374(3) . ?
C14 C15 1.388(3) . ?
