#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:35:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179147 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/08/4310832.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_4310832
loop_
_publ_author_name
'Pauli Kofod'
'Pernille Harris'
_publ_section_title
;
 NMR Spectroscopic and X-ray Crystallographic Study of Methylcobalt(III)
 Compounds with Saturated Amine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2680
_journal_page_last               2688
_journal_paper_doi               10.1021/ic0302682
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C5 H19 Cl4 Co N4 Zn'
_chemical_formula_weight         401.34
_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            8
_cell_length_a                   9.406(2)
_cell_length_b                   12.070(3)
_cell_length_c                   24.719(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      19.37
_cell_volume                     2806.4(11)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'DREADD (Blessing, 1987)'
_computing_molecular_graphics    'OrtepII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11521
_diffrn_reflns_theta_full        34.95
_diffrn_reflns_theta_max         34.95
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  166.7
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    3.629
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         6157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0367P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                5049
_reflns_number_total             6157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0302682_s1_2.cif
_cod_data_source_block           pk41.abs
_cod_database_code               4310832
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.92237(2) 0.211641(16) 0.623873(8) 0.01391(5) Uani 1 1 d . . .
Cl1 Cl 1.09468(4) 0.16528(4) 0.684511(18) 0.01670(8) Uani 1 1 d . . .
Cl2 Cl 0.91620(5) 0.39261(3) 0.602276(19) 0.01883(8) Uani 1 1 d . . .
Cl3 Cl 0.70878(4) 0.17314(3) 0.666963(17) 0.01503(7) Uani 1 1 d . . .
Cl4 Cl 0.94275(6) 0.10086(4) 0.551593(18) 0.02226(9) Uani 1 1 d . . .
Co Co 0.49692(2) 0.281193(19) 0.633345(9) 0.01233(5) Uani 1 1 d . . .
N1 N 0.59093(16) 0.41717(13) 0.65717(6) 0.0157(3) Uani 1 1 d . . .
H1A H 0.540(3) 0.476(2) 0.6416(11) 0.024 Uiso 1 1 d . . .
H1B H 0.684(3) 0.424(2) 0.6434(10) 0.024 Uiso 1 1 d . . .
N2 N 0.41943(15) 0.27467(12) 0.70729(6) 0.0147(3) Uani 1 1 d . . .
H2A H 0.470(3) 0.225(2) 0.7231(10) 0.022 Uiso 1 1 d . . .
H2B H 0.326(3) 0.255(2) 0.7067(10) 0.022 Uiso 1 1 d . . .
N3 N 0.58014(18) 0.28575(15) 0.56065(6) 0.0188(3) Uani 1 1 d . . .
H3A H 0.543(3) 0.337(2) 0.5419(11) 0.028 Uiso 1 1 d . . .
H3B H 0.669(3) 0.304(2) 0.5622(11) 0.028 Uiso 1 1 d . . .
N4 N 0.40709(16) 0.14210(14) 0.60954(7) 0.0173(3) Uani 1 1 d . . .
H4A H 0.454(3) 0.085(2) 0.6232(10) 0.026 Uiso 1 1 d . . .
H4B H 0.318(3) 0.136(2) 0.6185(10) 0.026 Uiso 1 1 d . . .
C1 C 0.58815(18) 0.42228(15) 0.71708(7) 0.0165(3) Uani 1 1 d . . .
H11 H 0.665(3) 0.367(2) 0.7289(10) 0.021 Uiso 1 1 d . . .
H12 H 0.608(3) 0.502(2) 0.7297(10) 0.021 Uiso 1 1 d . . .
C2 C 0.44309(19) 0.38269(15) 0.73477(8) 0.0166(3) Uani 1 1 d . . .
H21 H 0.435(3) 0.379(2) 0.7725(10) 0.022 Uiso 1 1 d . . .
H22 H 0.372(3) 0.436(2) 0.7207(9) 0.022 Uiso 1 1 d . . .
C3 C 0.5621(2) 0.17613(19) 0.53396(8) 0.0223(4) Uani 1 1 d . . .
H31 H 0.569(3) 0.184(2) 0.4977(11) 0.029 Uiso 1 1 d . . .
H32 H 0.635(3) 0.127(2) 0.5479(10) 0.029 Uiso 1 1 d . . .
C4 C 0.4163(2) 0.13403(18) 0.54987(8) 0.0220(4) Uani 1 1 d . . .
H41 H 0.345(3) 0.179(2) 0.5339(11) 0.029 Uiso 1 1 d . . .
H42 H 0.397(3) 0.061(2) 0.5355(11) 0.029 Uiso 1 1 d . . .
C5 C 0.32846(19) 0.36614(16) 0.60910(8) 0.0195(3) Uani 1 1 d . . .
H51 H 0.293(3) 0.404(2) 0.6357(10) 0.025 Uiso 1 1 d . . .
H52 H 0.347(3) 0.417(2) 0.5792(11) 0.025 Uiso 1 1 d . . .
H53 H 0.266(3) 0.325(2) 0.5958(10) 0.025 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'
Co Co 0.3494 0.9721 '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'
Cl Cl 0.1484 0.1585 '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
Cl4 Zn Cl2 113.12(2) . . ?
Cl4 Zn Cl1 108.51(2) . . ?
Cl2 Zn Cl1 114.402(18) . . ?
Cl4 Zn Cl3 108.70(2) . . ?
Cl2 Zn Cl3 106.324(17) . . ?
Cl1 Zn Cl3 105.35(2) . . ?
Zn Cl3 Co 115.41(2) . . ?
N1 Co N3 94.12(7) . . ?
N1 Co N2 85.49(6) . . ?
N3 Co N2 178.07(7) . . ?
N1 Co N4 178.47(6) . . ?
N3 Co N4 85.49(7) . . ?
N2 Co N4 94.85(7) . . ?
N1 Co C5 91.05(8) . . ?
N3 Co C5 91.58(8) . . ?
N2 Co C5 90.31(8) . . ?
N4 Co C5 90.44(8) . . ?
N1 Co Cl3 88.71(5) . . ?
N3 Co Cl3 90.06(5) . . ?
N2 Co Cl3 88.05(5) . . ?
N4 Co Cl3 89.81(5) . . ?
C5 Co Cl3 178.36(6) . . ?
C1 N1 Co 109.13(11) . . ?
C2 N2 Co 109.49(11) . . ?
C3 N3 Co 109.63(12) . . ?
C4 N4 Co 109.18(12) . . ?
N1 C1 C2 106.98(14) . . ?
N2 C2 C1 106.28(14) . . ?
N3 C3 C4 106.64(16) . . ?
N4 C4 C3 106.84(15) . . ?
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
Zn Cl4 2.2398(6) . ?
Zn Cl2 2.2494(7) . ?
Zn Cl1 2.2774(6) . ?
Zn Cl3 2.3209(6) . ?
Cl3 Co 2.5225(6) . ?
Co N1 1.9551(16) . ?
Co N3 1.9608(17) . ?
Co N2 1.9694(16) . ?
Co N4 1.9695(17) . ?
Co C5 1.9801(18) . ?
N1 C1 1.483(2) . ?
N2 C2 1.487(2) . ?
N3 C3 1.488(3) . ?
N4 C4 1.481(3) . ?
C1 C2 1.510(2) . ?
C3 C4 1.514(3) . ?
