#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:13:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179099 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/61/4306172.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_4306172
loop_
_publ_author_name
'Tyler J. Morin'
'Brian Bennett'
'Sergey V. Lindeman'
'James R. Gardinier'
_publ_section_title
;
First-Row Transition-Metal Complexes of a New Pentadentate Ligand,
α,α,α',α'-Tetra(pyrazolyl)lutidine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7468
_journal_page_last               7470
_journal_paper_doi               10.1021/ic801093q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C20 H19 Cl4 Co N9'
_chemical_formula_weight         586.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.0330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2900(2)
_cell_length_b                   19.1675(3)
_cell_length_c                   12.0572(2)
_cell_measurement_reflns_used    6674
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66
_cell_measurement_theta_min      4
_cell_volume                     2378.08(7)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_data_reduction        'SADABS-2004/1 (Bruker, 2005)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)'
_computing_structure_solution    'XS/SHELXTL v6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18513
_diffrn_reflns_theta_full        67.30
_diffrn_reflns_theta_max         67.30
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    10.046
_exptl_absorpt_correction_T_max  0.2963
_exptl_absorpt_correction_T_min  0.0725
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical (based on real shape of the crystal) absorption
 correction followed by:
 SADABS. Program for empirical absorption correction of
 area-detector data. University of Goetingen. Germany. 
 Sheldrick, G. M. 1996
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.00083(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0729P)²+2.7860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                4026
_reflns_number_total             4110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801093q_si_002_3.cif
_cod_data_source_block           CoClpz4lut_gard3sa
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4306172
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Co1 Co 0.49174(7) 0.12530(3) 0.30107(5) 0.01249(17) Uani 1 1 d . . .
Cl1 Cl 0.50363(11) 0.14352(5) 0.49126(7) 0.0212(2) Uani 1 1 d . . .
N1 N 0.4803(3) 0.10782(15) 0.1192(2) 0.0133(6) Uani 1 1 d . . .
N2 N 0.3244(3) 0.18883(16) 0.2711(3) 0.0153(7) Uani 1 1 d . . .
N3 N 0.2326(3) 0.16511(16) 0.1986(3) 0.0136(6) Uani 1 1 d . . .
N4 N 0.3548(3) 0.04144(17) 0.3015(3) 0.0153(7) Uani 1 1 d . . .
N5 N 0.2551(3) 0.04220(16) 0.2260(3) 0.0154(7) Uani 1 1 d . . .
N6 N 0.6302(3) 0.20349(17) 0.2541(3) 0.0166(7) Uani 1 1 d . . .
N7 N 0.7134(3) 0.18938(17) 0.1689(3) 0.0162(7) Uani 1 1 d . . .
N8 N 0.6578(3) 0.05576(16) 0.2853(3) 0.0154(7) Uani 1 1 d . . .
N9 N 0.7414(3) 0.06747(16) 0.1998(3) 0.0145(6) Uani 1 1 d . . .
C1 C 0.3652(4) 0.09717(18) 0.0699(3) 0.0133(8) Uani 1 1 d . . .
C2 C 0.3544(4) 0.08523(19) -0.0430(3) 0.0169(8) Uani 1 1 d . . .
H2A H 0.2716 0.0786 -0.0763 0.020 Uiso 1 1 calc R . .
C3 C 0.4668(4) 0.08317(19) -0.1068(3) 0.0186(8) Uani 1 1 d . . .
H3A H 0.4622 0.0742 -0.1842 0.022 Uiso 1 1 calc R . .
C4 C 0.5862(4) 0.09439(18) -0.0555(3) 0.0175(8) Uani 1 1 d . . .
H4A H 0.6646 0.0935 -0.0971 0.021 Uiso 1 1 calc R . .
C5 C 0.5882(4) 0.10688(19) 0.0573(3) 0.0134(7) Uani 1 1 d . . .
C6 C 0.2469(4) 0.09827(19) 0.1453(3) 0.0150(8) Uani 1 1 d . . .
H6A H 0.1682 0.0900 0.0984 0.018 Uiso 1 1 calc R . .
C7 C 0.7143(4) 0.12105(18) 0.1177(3) 0.0144(8) Uani 1 1 d . . .
H7A H 0.7861 0.1202 0.0619 0.017 Uiso 1 1 calc R . .
C8 C 0.2825(4) 0.2517(2) 0.3022(3) 0.0168(8) Uani 1 1 d . . .
H8A H 0.3262 0.2809 0.3538 0.020 Uiso 1 1 calc R . .
C9 C 0.1660(4) 0.2690(2) 0.2491(4) 0.0215(9) Uani 1 1 d . . .
H9A H 0.1173 0.3108 0.2570 0.026 Uiso 1 1 calc R . .
C10 C 0.1369(4) 0.2123(2) 0.1828(3) 0.0181(8) Uani 1 1 d . . .
H10A H 0.0638 0.2074 0.1353 0.022 Uiso 1 1 calc R . .
C11 C 0.3391(4) -0.0173(2) 0.3580(3) 0.0192(8) Uani 1 1 d . . .
H11A H 0.3936 -0.0319 0.4172 0.023 Uiso 1 1 calc R . .
C12 C 0.2314(4) -0.0551(2) 0.3190(3) 0.0206(8) Uani 1 1 d . . .
H12A H 0.2008 -0.0988 0.3452 0.025 Uiso 1 1 calc R . .
C13 C 0.1798(4) -0.0155(2) 0.2349(3) 0.0177(8) Uani 1 1 d . . .
H13A H 0.1055 -0.0264 0.1913 0.021 Uiso 1 1 calc R . .
C14 C 0.6547(4) 0.2694(2) 0.2822(4) 0.0203(9) Uani 1 1 d . . .
H14A H 0.6116 0.2939 0.3399 0.024 Uiso 1 1 calc R . .
C15 C 0.7529(4) 0.2978(2) 0.2149(4) 0.0233(9) Uani 1 1 d . . .
H15A H 0.7879 0.3436 0.2185 0.028 Uiso 1 1 calc R . .
C16 C 0.7877(4) 0.2457(2) 0.1430(3) 0.0185(8) Uani 1 1 d . . .
H16A H 0.8514 0.2484 0.0861 0.022 Uiso 1 1 calc R . .
C17 C 0.7104(4) 0.00285(19) 0.3415(3) 0.0172(8) Uani 1 1 d . . .
H17A H 0.6746 -0.0169 0.4070 0.021 Uiso 1 1 calc R . .
C18 C 0.8251(4) -0.0197(2) 0.2910(4) 0.0216(9) Uani 1 1 d . . .
H18A H 0.8797 -0.0568 0.3144 0.026 Uiso 1 1 calc R . .
C19 C 0.8428(4) 0.0227(2) 0.2013(3) 0.0184(8) Uani 1 1 d . . .
H19A H 0.9127 0.0210 0.1499 0.022 Uiso 1 1 calc R . .
Cl2 Cl 0.98847(9) 0.11019(4) -0.03561(7) 0.0165(2) Uani 1 1 d . . .
Cl1S Cl 0.42952(12) 0.27316(6) 0.03607(11) 0.0376(3) Uani 1 1 d . . .
Cl2S Cl 0.53787(16) 0.39565(7) -0.06953(12) 0.0519(4) Uani 1 1 d . . .
C1S C 0.4123(5) 0.3331(3) -0.0734(4) 0.0333(11) Uani 1 1 d . . .
H1SA H 0.3271 0.3568 -0.0675 0.040 Uiso 1 1 calc R . .
H1SB H 0.4148 0.3079 -0.1451 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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
N4 Co1 N2 84.13(12) . . ?
N4 Co1 N6 164.63(13) . . ?
N2 Co1 N6 95.31(12) . . ?
N4 Co1 N8 93.28(12) . . ?
N2 Co1 N8 165.02(12) . . ?
N6 Co1 N8 83.29(12) . . ?
N4 Co1 N1 81.62(12) . . ?
N2 Co1 N1 82.94(12) . . ?
N6 Co1 N1 83.07(12) . . ?
N8 Co1 N1 82.09(12) . . ?
N4 Co1 Cl1 98.35(9) . . ?
N2 Co1 Cl1 97.06(9) . . ?
N6 Co1 Cl1 96.96(9) . . ?
N8 Co1 Cl1 97.91(9) . . ?
N1 Co1 Cl1 179.97(12) . . ?
C5 N1 C1 118.9(3) . . ?
C5 N1 Co1 120.6(2) . . ?
C1 N1 Co1 120.5(3) . . ?
C8 N2 N3 104.9(3) . . ?
C8 N2 Co1 136.6(3) . . ?
N3 N2 Co1 118.4(2) . . ?
C10 N3 N2 111.8(3) . . ?
C10 N3 C6 127.4(3) . . ?
N2 N3 C6 120.7(3) . . ?
C11 N4 N5 105.0(3) . . ?
C11 N4 Co1 136.1(3) . . ?
N5 N4 Co1 118.9(2) . . ?
C13 N5 N4 111.5(3) . . ?
C13 N5 C6 128.6(3) . . ?
N4 N5 C6 119.7(3) . . ?
C14 N6 N7 105.1(3) . . ?
C14 N6 Co1 136.2(3) . . ?
N7 N6 Co1 118.5(2) . . ?
C16 N7 N6 111.7(3) . . ?
C16 N7 C7 128.1(3) . . ?
N6 N7 C7 120.3(3) . . ?
C17 N8 N9 104.7(3) . . ?
C17 N8 Co1 137.7(3) . . ?
N9 N8 Co1 117.5(2) . . ?
C19 N9 N8 111.9(3) . . ?
C19 N9 C7 127.3(3) . . ?
N8 N9 C7 120.7(3) . . ?
N1 C1 C2 122.1(4) . . ?
N1 C1 C6 116.1(3) . . ?
C2 C1 C6 121.7(3) . . ?
C1 C2 C3 118.8(4) . . ?
C2 C3 C4 119.0(3) . . ?
C5 C4 C3 118.5(4) . . ?
N1 C5 C4 122.7(4) . . ?
N1 C5 C7 116.1(3) . . ?
C4 C5 C7 121.2(4) . . ?
N3 C6 N5 111.4(3) . . ?
N3 C6 C1 111.2(3) . . ?
N5 C6 C1 110.1(3) . . ?
N7 C7 N9 110.5(3) . . ?
N7 C7 C5 111.2(3) . . ?
N9 C7 C5 111.4(3) . . ?
N2 C8 C9 111.3(3) . . ?
C10 C9 C8 105.2(3) . . ?
N3 C10 C9 106.7(3) . . ?
N4 C11 C12 111.3(4) . . ?
C13 C12 C11 105.5(3) . . ?
N5 C13 C12 106.7(3) . . ?
N6 C14 C15 110.9(4) . . ?
C16 C15 C14 105.7(3) . . ?
N7 C16 C15 106.6(4) . . ?
N8 C17 C18 110.8(4) . . ?
C19 C18 C17 105.9(3) . . ?
N9 C19 C18 106.6(4) . . ?
Cl1S C1S Cl2S 110.5(3) . . ?
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
Co1 N4 2.138(3) . ?
Co1 N2 2.140(3) . ?
Co1 N6 2.144(3) . ?
Co1 N8 2.175(3) . ?
Co1 N1 2.221(3) . ?
Co1 Cl1 2.3228(10) . ?
N1 C5 1.338(5) . ?
N1 C1 1.340(5) . ?
N2 C8 1.333(5) . ?
N2 N3 1.365(4) . ?
N3 C10 1.350(5) . ?
N3 C6 1.441(5) . ?
N4 C11 1.326(5) . ?
N4 N5 1.371(4) . ?
N5 C13 1.355(5) . ?
N5 C6 1.452(5) . ?
N6 C14 1.331(5) . ?
N6 N7 1.365(5) . ?
N7 C16 1.359(5) . ?
N7 C7 1.448(5) . ?
N8 C17 1.334(5) . ?
N8 N9 1.362(5) . ?
N9 C19 1.351(5) . ?
N9 C7 1.453(5) . ?
C1 C2 1.385(5) . ?
C1 C6 1.520(6) . ?
C2 C3 1.389(6) . ?
C3 C4 1.392(6) . ?
C4 C5 1.381(6) . ?
C5 C7 1.513(5) . ?
C8 C9 1.399(6) . ?
C9 C10 1.382(6) . ?
C11 C12 1.404(6) . ?
C12 C13 1.374(6) . ?
C14 C15 1.407(6) . ?
C15 C16 1.370(6) . ?
C17 C18 1.397(6) . ?
C18 C19 1.365(6) . ?
Cl1S C1S 1.758(5) . ?
Cl2S C1S 1.764(5) . ?
