#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:19:13 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179104 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/66/4306625.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_4306625
loop_
_publ_author_name
'Annekathrin Seifert'
'Gerald Linti'
_publ_contact_author_address
;University of Heidelberg
Institute of Inorganic Chemistry
Im Neuenheimer Feld 270
D-69120 Heidelberg
Germany
;
_publ_contact_author_email       gerald.linti@aci.uni-hedielberg.de
_publ_contact_author_fax         Int+6221546617
_publ_contact_author_name        'Gerald Linti'
_publ_contact_author_phone       Int+6221548468
_publ_section_title
;
2,2,6,6-Tetramethylpiperidinogallium as a Terminal and Bridging Ligand in
Homo- and Heteroleptic Chromium, Nickel, and Cobalt Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11398
_journal_page_last               11404
_journal_paper_doi               10.1021/ic801437n
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C24 H36 Co2 Ga2 N2 O6'
_chemical_formula_weight         705.85
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 96.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6708(19)
_cell_length_b                   10.629(2)
_cell_length_c                   14.655(3)
_cell_measurement_temperature    200(2)
_cell_volume                     1496.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9615
_diffrn_reflns_theta_full        24.02
_diffrn_reflns_theta_max         24.02
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.908
_exptl_absorpt_correction_T_max  .68
_exptl_absorpt_correction_T_min  .67
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .18
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4669
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0681P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                4211
_reflns_number_total             4669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801437n_si_001_3.cif
_cod_data_source_block           aks82_comp_4
_cod_original_cell_volume        1496.2(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4306625
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 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
Ga1 Ga 1.84798(6) -0.05959(6) 0.28862(4) 0.02760(17) Uani 1 1 d . . .
Ga2 Ga 1.63561(7) 0.15327(6) 0.30324(4) 0.02678(17) Uani 1 1 d . . .
Co2 Co 1.61707(8) -0.06425(9) 0.33173(5) 0.0287(2) Uani 1 1 d . . .
Co1 Co 1.83797(8) 0.09802(8) 0.39986(6) 0.0295(2) Uani 1 1 d . . .
N1 N 1.9602(6) -0.1383(5) 0.2117(4) 0.0314(12) Uani 1 1 d . . .
N2 N 1.5503(6) 0.2847(5) 0.2375(4) 0.0307(12) Uani 1 1 d . . .
O19 O 2.0781(6) -0.0390(7) 0.4929(4) 0.0609(17) Uani 1 1 d . . .
O20 O 1.9697(7) 0.3168(6) 0.3220(5) 0.0628(16) Uani 1 1 d . . .
O21 O 1.6946(6) 0.1680(7) 0.5596(4) 0.0617(16) Uani 1 1 d . . .
O22 O 1.5361(6) -0.1667(6) 0.1480(4) 0.0516(14) Uani 1 1 d . . .
O23 O 1.3424(6) 0.0071(7) 0.3817(5) 0.0656(17) Uani 1 1 d . . .
O24 O 1.6917(9) -0.2630(7) 0.4707(5) 0.085(2) Uani 1 1 d . . .
C1 C 1.9754(8) -0.2784(7) 0.2158(5) 0.0370(15) Uani 1 1 d . . .
C2 C 2.1245(8) -0.3142(7) 0.2021(5) 0.0458(19) Uani 1 1 d . . .
H2A H 2.1872 -0.2880 0.2571 0.055 Uiso 1 1 calc R . .
H2B H 2.1306 -0.4068 0.1972 0.055 Uiso 1 1 calc R . .
C3 C 2.1755(8) -0.2554(8) 0.1177(6) 0.0453(18) Uani 1 1 d . . .
H3A H 2.1179 -0.2853 0.0617 0.054 Uiso 1 1 calc R . .
H3B H 2.2732 -0.2808 0.1137 0.054 Uiso 1 1 calc R . .
C4 C 2.1661(7) -0.1107(8) 0.1241(6) 0.0429(18) Uani 1 1 d . . .
H4A H 2.1951 -0.0730 0.0675 0.051 Uiso 1 1 calc R . .
H4B H 2.2313 -0.0810 0.1767 0.051 Uiso 1 1 calc R . .
C5 C 2.0163(6) -0.0651(7) 0.1363(4) 0.0336(14) Uani 1 1 d . . .
C6 C 1.8696(8) -0.3470(9) 0.1449(6) 0.0498(18) Uani 1 1 d . . .
H6A H 1.8938 -0.3315 0.0828 0.075 Uiso 1 1 calc R . .
H6B H 1.7756 -0.3152 0.1498 0.075 Uiso 1 1 calc R . .
H6C H 1.8725 -0.4376 0.1574 0.075 Uiso 1 1 calc R . .
C7 C 1.9473(11) -0.3217(8) 0.3128(6) 0.061(2) Uani 1 1 d . . .
H7A H 2.0111 -0.2780 0.3591 0.091 Uiso 1 1 calc R . .
H7B H 1.9622 -0.4127 0.3186 0.091 Uiso 1 1 calc R . .
H7C H 1.8510 -0.3017 0.3220 0.091 Uiso 1 1 calc R . .
C8 C 1.9204(8) -0.0726(8) 0.0444(5) 0.0466(17) Uani 1 1 d . . .
H8A H 1.8272 -0.0423 0.0535 0.070 Uiso 1 1 calc R . .
H8B H 1.9144 -0.1600 0.0231 0.070 Uiso 1 1 calc R . .
H8C H 1.9587 -0.0201 -0.0016 0.070 Uiso 1 1 calc R . .
C9 C 2.0286(8) 0.0744(7) 0.1651(6) 0.0443(18) Uani 1 1 d . . .
H9A H 1.9360 0.1077 0.1723 0.066 Uiso 1 1 calc R . .
H9B H 2.0692 0.1226 0.1178 0.066 Uiso 1 1 calc R . .
H9C H 2.0885 0.0816 0.2236 0.066 Uiso 1 1 calc R . .
C10 C 1.4776(7) 0.3853(7) 0.2853(5) 0.0353(15) Uani 1 1 d . . .
C11 C 1.4982(8) 0.5140(6) 0.2397(5) 0.0388(16) Uani 1 1 d . . .
H11A H 1.4406 0.5781 0.2666 0.047 Uiso 1 1 calc R . .
H11B H 1.5969 0.5397 0.2529 0.047 Uiso 1 1 calc R . .
C12 C 1.4581(8) 0.5093(7) 0.1352(5) 0.0436(17) Uani 1 1 d . . .
H12A H 1.3578 0.4897 0.1214 0.052 Uiso 1 1 calc R . .
H12B H 1.4754 0.5922 0.1079 0.052 Uiso 1 1 calc R . .
C13 C 1.5443(8) 0.4083(6) 0.0936(5) 0.0381(16) Uani 1 1 d . . .
H13A H 1.6437 0.4331 0.1029 0.046 Uiso 1 1 calc R . .
H13B H 1.5157 0.4042 0.0266 0.046 Uiso 1 1 calc R . .
C14 C 1.5290(7) 0.2758(6) 0.1353(4) 0.0319(14) Uani 1 1 d . . .
C15 C 1.3216(8) 0.3575(8) 0.2905(6) 0.0458(18) Uani 1 1 d . . .
H15A H 1.2694 0.3695 0.2298 0.069 Uiso 1 1 calc R . .
H15B H 1.2859 0.4149 0.3346 0.069 Uiso 1 1 calc R . .
H15C H 1.3109 0.2704 0.3105 0.069 Uiso 1 1 calc R . .
C16 C 1.5491(9) 0.3919(8) 0.3848(5) 0.052(2) Uani 1 1 d . . .
H16A H 1.6494 0.4046 0.3842 0.077 Uiso 1 1 calc R . .
H16B H 1.5331 0.3130 0.4167 0.077 Uiso 1 1 calc R . .
H16C H 1.5103 0.4622 0.4169 0.077 Uiso 1 1 calc R . .
C17 C 1.3869(8) 0.2155(8) 0.0979(5) 0.0482(19) Uani 1 1 d . . .
H17A H 1.3724 0.1388 0.1326 0.072 Uiso 1 1 calc R . .
H17B H 1.3873 0.1946 0.0328 0.072 Uiso 1 1 calc R . .
H17C H 1.3116 0.2752 0.1047 0.072 Uiso 1 1 calc R . .
C18 C 1.6455(8) 0.1917(8) 0.1049(5) 0.0432(17) Uani 1 1 d . . .
H18A H 1.7364 0.2272 0.1281 0.065 Uiso 1 1 calc R . .
H18B H 1.6369 0.1879 0.0377 0.065 Uiso 1 1 calc R . .
H18C H 1.6374 0.1068 0.1298 0.065 Uiso 1 1 calc R . .
C19 C 1.9828(8) 0.0119(8) 0.4566(5) 0.0430(18) Uani 1 1 d . . .
C20 C 1.9148(8) 0.2309(7) 0.3497(5) 0.0415(17) Uani 1 1 d . . .
C21 C 1.7500(8) 0.1414(8) 0.4963(5) 0.0441(17) Uani 1 1 d . . .
C22 C 1.5735(7) -0.1249(7) 0.2204(5) 0.0334(15) Uani 1 1 d . . .
C23 C 1.4525(7) -0.0157(8) 0.3648(5) 0.0406(17) Uani 1 1 d . . .
C24 C 1.6626(9) -0.1854(9) 0.4168(6) 0.055(2) Uani 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'
Ga Ga 0.2307 1.6083 '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'
O O 0.0106 0.0060 '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
N1 Ga1 Co1 144.98(18) . . ?
N1 Ga1 Co2 141.49(18) . . ?
Co1 Ga1 Co2 73.53(4) . . ?
N2 Ga2 Co1 142.84(18) . . ?
N2 Ga2 Co2 143.02(18) . . ?
Co1 Ga2 Co2 73.98(4) . . ?
C22 Co2 C23 103.4(3) . . ?
C22 Co2 C24 113.0(4) . . ?
C23 Co2 C24 99.9(4) . . ?
C22 Co2 Ga2 102.1(2) . . ?
C23 Co2 Ga2 81.6(3) . . ?
C24 Co2 Ga2 143.2(3) . . ?
C22 Co2 Ga1 83.9(2) . . ?
C23 Co2 Ga1 162.1(3) . . ?
C24 Co2 Ga1 92.1(3) . . ?
Ga2 Co2 Ga1 80.82(3) . . ?
C22 Co2 Co1 129.7(2) . . ?
C23 Co2 Co1 112.7(3) . . ?
C24 Co2 Co1 94.4(3) . . ?
Ga2 Co2 Co1 52.91(3) . . ?
Ga1 Co2 Co1 52.54(3) . . ?
C21 Co1 C20 112.2(4) . . ?
C21 Co1 C19 100.5(3) . . ?
C20 Co1 C19 104.7(4) . . ?
C21 Co1 Ga1 142.4(3) . . ?
C20 Co1 Ga1 103.0(2) . . ?
C19 Co1 Ga1 82.3(2) . . ?
C21 Co1 Ga2 88.4(2) . . ?
C20 Co1 Ga2 84.9(3) . . ?
C19 Co1 Ga2 163.0(3) . . ?
Ga1 Co1 Ga2 81.86(4) . . ?
C21 Co1 Co2 91.6(3) . . ?
C20 Co1 Co2 131.7(3) . . ?
C19 Co1 Co2 111.6(3) . . ?
Ga1 Co1 Co2 53.94(3) . . ?
Ga2 Co1 Co2 53.11(3) . . ?
C1 N1 C5 120.2(5) . . ?
C1 N1 Ga1 119.1(4) . . ?
C5 N1 Ga1 120.0(4) . . ?
C14 N2 C10 119.8(5) . . ?
C14 N2 Ga2 118.7(4) . . ?
C10 N2 Ga2 120.3(4) . . ?
N1 C1 C2 109.4(6) . . ?
N1 C1 C7 107.8(6) . . ?
C2 C1 C7 108.4(6) . . ?
N1 C1 C6 112.7(6) . . ?
C2 C1 C6 110.8(6) . . ?
C7 C1 C6 107.7(7) . . ?
C3 C2 C1 113.9(6) . . ?
C2 C3 C4 109.5(6) . . ?
C3 C4 C5 112.3(6) . . ?
N1 C5 C9 108.6(5) . . ?
N1 C5 C8 112.5(5) . . ?
C9 C5 C8 107.9(6) . . ?
N1 C5 C4 110.1(6) . . ?
C9 C5 C4 106.7(6) . . ?
C8 C5 C4 110.9(6) . . ?
N2 C10 C16 106.9(5) . . ?
N2 C10 C11 109.8(5) . . ?
C16 C10 C11 107.6(7) . . ?
N2 C10 C15 113.5(6) . . ?
C16 C10 C15 107.2(6) . . ?
C11 C10 C15 111.5(6) . . ?
C12 C11 C10 111.8(6) . . ?
C13 C12 C11 109.5(6) . . ?
C12 C13 C14 113.5(5) . . ?
N2 C14 C18 107.8(5) . . ?
N2 C14 C13 109.3(5) . . ?
C18 C14 C13 107.8(5) . . ?
N2 C14 C17 113.2(6) . . ?
C18 C14 C17 107.7(6) . . ?
C13 C14 C17 110.9(6) . . ?
O19 C19 Co1 177.5(8) . . ?
O20 C20 Co1 176.0(7) . . ?
O21 C21 Co1 178.9(7) . . ?
O22 C22 Co2 175.7(6) . . ?
O23 C23 Co2 174.3(7) . . ?
O24 C24 Co2 179.7(8) . . ?
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
Ga1 N1 1.853(5) . ?
Ga1 Co1 2.3472(11) . ?
Ga1 Co2 2.3905(11) . ?
Ga2 N2 1.838(6) . ?
Ga2 Co1 2.3535(13) . ?
Ga2 Co2 2.3599(12) . ?
Co2 C22 1.759(7) . ?
Co2 C23 1.793(7) . ?
Co2 C24 1.812(10) . ?
Co2 Co1 2.8358(13) . ?
Co1 C21 1.793(7) . ?
Co1 C20 1.793(8) . ?
Co1 C19 1.795(8) . ?
N1 C1 1.498(9) . ?
N1 C5 1.502(8) . ?
N2 C14 1.491(8) . ?
N2 C10 1.498(9) . ?
O19 C19 1.146(9) . ?
O20 C20 1.153(10) . ?
O21 C21 1.158(9) . ?
O22 C22 1.169(9) . ?
O23 C23 1.146(9) . ?
O24 C24 1.153(11) . ?
C1 C2 1.527(10) . ?
C1 C7 1.547(10) . ?
C1 C6 1.553(11) . ?
C2 C3 1.518(11) . ?
C3 C4 1.544(11) . ?
C4 C5 1.558(9) . ?
C5 C9 1.543(11) . ?
C5 C8 1.547(10) . ?
C10 C16 1.542(10) . ?
C10 C11 1.545(10) . ?
C10 C15 1.547(10) . ?
C11 C12 1.537(11) . ?
C12 C13 1.529(10) . ?
C13 C14 1.549(10) . ?
C14 C18 1.543(10) . ?
C14 C17 1.557(10) . ?
