#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/68/4106835.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_4106835
loop_
_publ_author_name
'Guang-Peng Wu'
'Sheng-Hsuan Wei'
'Wei-Min Ren'
'Xiao-Bing Lu'
'Tie-Qi Xu'
'Donald J. Darensbourg'
_publ_section_title
;
 Perfectly Alternating Copolymerization of CO2 and Epichlorohydrin Using
 Cobalt(III)-Based Catalyst Systems
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15191
_journal_page_last               15199
_journal_paper_doi               10.1021/ja206425j
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C13 H28 Cl4 Co0.5 N3 O6'
_chemical_formula_weight         493.65
_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                102.990(3)
_cell_angle_beta                 98.340(3)
_cell_angle_gamma                90.483(3)
_cell_formula_units_Z            2
_cell_length_a                   5.9712(3)
_cell_length_b                   11.2350(5)
_cell_length_c                   16.7877(8)
_cell_measurement_reflns_used    10999
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      1.86
_cell_volume                     1084.82(9)
_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      273(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       ω-2θ
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10999
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             513
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.720
_refine_diff_density_min         -4.570
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.818
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.818
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.1273
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4067
_refine_ls_wR_factor_ref         0.4448
_reflns_number_gt                3550
_reflns_number_total             4838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja206425j_si_003.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C13 H28 Cl4 Co0.50 N3 O6'
_cod_database_code               4106835
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
Co1 Co 0.0000 0.5000 0.5000 0.0853(9) Uani 1 2 d S
Cl3 Cl 0.7154(3) 0.53655(17) 0.71657(10) 0.0343(5) Uani 1 1 d .
Cl4 Cl 0.5610(3) 0.6995(2) 0.99548(13) 0.0505(7) Uani 1 1 d .
Cl5 Cl 0.9290(4) 0.8383(2) 0.95735(16) 0.0526(7) Uani 1 1 d .
Cl2 Cl 0.5615(3) 0.19326(15) 0.45305(13) 0.0356(6) Uani 1 1 d .
O6 O 0.2831(8) 0.5638(5) 0.5884(3) 0.0327(12) Uani 1 1 d .
O4 O -0.0883(7) 0.3801(4) 0.5692(3) 0.0258(10) Uani 1 1 d .
O2 O 0.0465(7) 0.3027(4) 0.7971(3) 0.0300(11) Uani 1 1 d .
O1 O -0.1488(8) 0.3764(5) 0.8988(3) 0.0381(13) Uani 1 1 d .
O3 O 0.1351(8) 0.4882(4) 0.8746(3) 0.0324(12) Uani 1 1 d .
O5 O 0.1640(7) 0.3617(4) 0.4311(3) 0.0282(11) Uani 1 1 d .
N1 N 0.3440(9) 0.1391(5) 0.7051(3) 0.0244(12) Uani 1 1 d .
C9 C 0.4141(10) 0.2635(6) 0.7534(4) 0.0249(14) Uani 1 1 d .
H9A H 0.5303 0.2960 0.7284 0.030 Uiso 1 1 calc R
H9B H 0.4807 0.2590 0.8088 0.030 Uiso 1 1 calc R
N2 N 0.4379(9) 0.0472(5) 0.8161(3) 0.0251(12) Uani 1 1 d .
N3 N 0.1458(9) -0.0374(5) 0.7109(3) 0.0247(12) Uani 1 1 d .
C4 C 0.3100(10) 0.0482(5) 0.7436(4) 0.0203(12) Uani 1 1 d .
C12 C -0.0020(11) 0.3894(6) 0.8608(4) 0.0280(15) Uani 1 1 d .
C1 C 0.2294(13) 0.1244(7) 0.6185(4) 0.0343(16) Uani 1 1 d .
H1A H 0.3001 0.0615 0.5818 0.041 Uiso 1 1 calc R
H1B H 0.2422 0.2005 0.6010 0.041 Uiso 1 1 calc R
C11 C 0.2930(12) 0.4738(6) 0.8170(5) 0.0336(16) Uani 1 1 d .
H11A H 0.4470 0.4738 0.8450 0.040 Uiso 1 1 calc R
H11B H 0.2821 0.5387 0.7872 0.040 Uiso 1 1 calc R
C7 C 0.3664(13) -0.0416(7) 0.8621(4) 0.0323(15) Uani 1 1 d .
H7A H 0.2275 -0.0167 0.8836 0.039 Uiso 1 1 calc R
H7B H 0.4826 -0.0447 0.9084 0.039 Uiso 1 1 calc R
C6 C 0.3293(14) -0.1650(7) 0.8039(5) 0.0386(18) Uani 1 1 d .
H6A H 0.4669 -0.1889 0.7811 0.046 Uiso 1 1 calc R
H6B H 0.2893 -0.2256 0.8330 0.046 Uiso 1 1 calc R
C10 C 0.2227(11) 0.3512(6) 0.7593(4) 0.0275(14) Uani 1 1 d .
H10 H 0.1601 0.3620 0.7042 0.033 Uiso 1 1 calc R
C8 C 0.6827(12) 0.0753(7) 0.8277(5) 0.0363(17) Uani 1 1 d .
H8A H 0.7612 0.0006 0.8161 0.054 Uiso 1 1 calc R
H8B H 0.7327 0.1184 0.8838 0.054 Uiso 1 1 calc R
H8C H 0.7142 0.1253 0.7909 0.054 Uiso 1 1 calc R
C3 C -0.0250(12) -0.0323(7) 0.6396(5) 0.0341(16) Uani 1 1 d .
H3A H -0.1745 -0.0455 0.6530 0.041 Uiso 1 1 calc R
H3B H -0.0021 -0.0976 0.5931 0.041 Uiso 1 1 calc R
C2 C -0.0141(14) 0.0893(7) 0.6148(5) 0.0383(18) Uani 1 1 d .
H2A H -0.0942 0.0818 0.5593 0.046 Uiso 1 1 calc R
H2B H -0.0843 0.1512 0.6523 0.046 Uiso 1 1 calc R
C13 C 0.7980(13) 0.6898(7) 0.9442(5) 0.0356(16) Uani 1 1 d .
H13A H 0.7519 0.6545 0.8857 0.043 Uiso 1 1 calc R
H13B H 0.9061 0.6369 0.9660 0.043 Uiso 1 1 calc R
C5 C 0.1420(13) -0.1575(6) 0.7360(5) 0.0333(16) Uani 1 1 d .
H5A H -0.0021 -0.1693 0.7541 0.040 Uiso 1 1 calc R
H5B H 0.1538 -0.2230 0.6883 0.040 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
O5 Co1 O5 180.000(1) 2_566 .
O5 Co1 O4 90.52(19) 2_566 .
O5 Co1 O4 89.48(19) . .
O5 Co1 O4 89.48(19) 2_566 2_566
O5 Co1 O4 90.52(19) . 2_566
O4 Co1 O4 180.000(1) . 2_566
O5 Co1 O6 84.9(2) 2_566 .
O5 Co1 O6 95.1(2) . .
O4 Co1 O6 90.25(18) . .
O4 Co1 O6 89.75(18) 2_566 .
O5 Co1 O6 95.1(2) 2_566 2_566
O5 Co1 O6 84.9(2) . 2_566
O4 Co1 O6 89.75(18) . 2_566
O4 Co1 O6 90.25(18) 2_566 2_566
O6 Co1 O6 180.000(1) . 2_566
C12 O2 C10 109.0(5) . .
C12 O3 C11 111.4(5) . .
C4 N1 C9 120.6(5) . .
C4 N1 C1 117.4(5) . .
C9 N1 C1 118.1(5) . .
N1 C9 C10 114.0(5) . .
C4 N2 C8 119.9(6) . .
C4 N2 C7 116.7(5) . .
C8 N2 C7 115.5(5) . .
C4 N3 C3 123.8(6) . .
C4 N3 C5 122.0(5) . .
C3 N3 C5 113.5(5) . .
N3 C4 N2 120.3(6) . .
N3 C4 N1 120.2(6) . .
N2 C4 N1 119.5(5) . .
O1 C12 O3 125.8(6) . .
O1 C12 O2 122.7(6) . .
O3 C12 O2 111.4(6) . .
N1 C1 C2 108.4(6) . .
O3 C11 C10 103.7(5) . .
N2 C7 C6 108.3(6) . .
C5 C6 C7 108.2(6) . .
O2 C10 C11 103.9(5) . .
O2 C10 C9 109.1(5) . .
C11 C10 C9 112.9(6) . .
N3 C3 C2 112.3(5) . .
C1 C2 C3 107.9(6) . .
Cl4 C13 Cl5 110.5(4) . .
C6 C5 N3 112.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O5 2.064(5) 2_566
Co1 O5 2.064(5) .
Co1 O4 2.076(4) .
Co1 O4 2.076(4) 2_566
Co1 O6 2.085(4) .
Co1 O6 2.085(4) 2_566
Cl4 C13 1.752(8) .
Cl5 C13 1.790(8) .
O2 C12 1.344(8) .
O2 C10 1.464(8) .
O1 C12 1.183(8) .
O3 C12 1.330(8) .
O3 C11 1.430(9) .
N1 C4 1.354(8) .
N1 C9 1.473(8) .
N1 C1 1.487(8) .
C9 C10 1.514(9) .
N2 C4 1.343(8) .
N2 C8 1.468(9) .
N2 C7 1.487(9) .
N3 C4 1.333(8) .
N3 C3 1.468(8) .
N3 C5 1.502(8) .
C1 C2 1.492(11) .
C11 C10 1.512(9) .
C7 C6 1.500(11) .
C6 C5 1.494(11) .
C3 C2 1.518(11) .
