#------------------------------------------------------------------------------
#$Date: 2019-11-23 02:16:15 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231856 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/65/4346584.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_4346584
loop_
_publ_author_name
'Przyojski, Jacob A.'
'Kiewit, Monica L.'
'Fillman, Kathlyn L.'
'Arman, Hadi D.'
'Tonzetich, Zachary J.'
_publ_section_related_literature
;
?
;
_publ_section_title
;
 Homoleptic transition metal complexes of the 7-azaindolide ligand
 featuring κ(1)-N1 coordination.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9637
_journal_page_last               9645
_journal_paper_doi               10.1021/acs.inorgchem.5b01732
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C28 H20 Co N8 Na2, 2(C7 H8)'
_chemical_formula_sum            'C42 H36 Co N8 Na2'
_chemical_formula_weight         757.70
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-16
_audit_creation_method           SHELXL-97
_audit_update_record
;
?

;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.757(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.867(4)
_cell_length_b                   11.515(3)
_cell_length_c                   21.666(7)
_cell_measurement_reflns_used    6978
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      2.5
_cell_volume                     3665.8(18)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11739
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.634
_refine_diff_density_rms         '0.071 ====END'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0500
_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)+(0.0650P)²+7.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                2915
_reflns_number_total             3413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01732_si_002.cif
_cod_data_source_block           Na2[Co(AzaIn)4]-2C7H8
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4346584
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Co1 Co 1.0000 0.29915(5) 0.7500 0.01640(17) Uani 1 2 d S
Na1 Na 0.92234(7) 0.48590(10) 0.64477(5) 0.0214(3) Uani 1 1 d .
N1 N 0.99606(15) 0.1938(2) 0.67634(11) 0.0181(5) Uani 1 1 d .
N2 N 0.90939(15) 0.2988(2) 0.59150(11) 0.0190(5) Uani 1 1 d .
N3 N 0.88360(15) 0.3904(2) 0.74221(11) 0.0191(5) Uani 1 1 d .
N4 N 0.91687(16) 0.5231(2) 0.82896(12) 0.0213(5) Uani 1 1 d .
C1 C 1.03304(19) 0.0836(3) 0.68043(14) 0.0208(6) Uani 1 1 d .
H1A H 1.0687 0.0540 0.7172 0.025 Uiso 1 1 calc R
C2 C 1.01329(19) 0.0209(3) 0.62618(14) 0.0213(6) Uani 1 1 d .
H2A H 1.0314 -0.0564 0.6189 0.026 Uiso 1 1 calc R
C3 C 0.95984(18) 0.0964(2) 0.58290(13) 0.0189(6) Uani 1 1 d .
C4 C 0.91648(18) 0.0899(3) 0.52140(14) 0.0206(6) Uani 1 1 d .
H4A H 0.9175 0.0204 0.4978 0.025 Uiso 1 1 calc R
C5 C 0.87187(19) 0.1879(3) 0.49576(14) 0.0224(6) Uani 1 1 d .
H5A H 0.8422 0.1868 0.4537 0.027 Uiso 1 1 calc R
C6 C 0.87034(19) 0.2892(3) 0.53161(14) 0.0200(6) Uani 1 1 d .
H6A H 0.8397 0.3552 0.5123 0.024 Uiso 1 1 calc R
C7 C 0.95270(18) 0.2022(2) 0.61619(13) 0.0170(6) Uani 1 1 d .
C8 C 0.80171(19) 0.3436(3) 0.71210(14) 0.0211(6) Uani 1 1 d .
H8A H 0.8024 0.2582 0.7038 0.025 Uiso 1 1 calc R
C9 C 0.72770(19) 0.3837(3) 0.73591(14) 0.0218(6) Uani 1 1 d .
H9A H 0.6658 0.3640 0.7222 0.026 Uiso 1 1 calc R
C10 C 0.76170(19) 0.4610(2) 0.78541(14) 0.0196(6) Uani 1 1 d .
C11 C 0.7249(2) 0.5267(3) 0.82988(14) 0.0224(6) Uani 1 1 d .
H11A H 0.6613 0.5275 0.8311 0.027 Uiso 1 1 calc R
C12 C 0.7845(2) 0.5902(3) 0.87192(14) 0.0231(6) Uani 1 1 d .
H12A H 0.7618 0.6365 0.9024 0.028 Uiso 1 1 calc R
C13 C 0.8779(2) 0.5867(3) 0.86982(14) 0.0242(7) Uani 1 1 d .
H13A H 0.9166 0.6324 0.8992 0.029 Uiso 1 1 calc R
C14 C 0.85780(19) 0.4622(2) 0.78782(13) 0.0179(6) Uani 1 1 d .
C15 C 0.8518(2) 0.6620(3) 0.53209(17) 0.0298(7) Uani 1 1 d .
C16 C 0.7793(2) 0.5911(3) 0.54240(17) 0.0303(7) Uani 1 1 d .
H16A H 0.7491 0.5403 0.5079 0.036 Uiso 1 1 calc R
C17 C 0.7480(2) 0.5904(3) 0.59968(18) 0.0359(8) Uani 1 1 d .
H17A H 0.6909 0.5473 0.6041 0.043 Uiso 1 1 calc R
C18 C 0.7885(2) 0.6609(3) 0.64829(18) 0.0384(8) Uani 1 1 d .
H18A H 0.7591 0.6714 0.6865 0.046 Uiso 1 1 calc R
C19 C 0.8606(3) 0.7318(3) 0.63820(19) 0.0412(9) Uani 1 1 d .
H19A H 0.8871 0.7876 0.6714 0.049 Uiso 1 1 calc R
C20 C 0.8915(2) 0.7321(3) 0.58093(18) 0.0346(8) Uani 1 1 d .
H20A H 0.9409 0.7812 0.5750 0.042 Uiso 1 1 calc R
C21 C 0.8849(2) 0.6627(3) 0.47016(18) 0.0398(9) Uani 1 1 d .
H21A H 0.8488 0.6082 0.4418 0.060 Uiso 1 1 calc R
H21B H 0.9491 0.6395 0.4758 0.060 Uiso 1 1 calc R
H21C H 0.8787 0.7411 0.4524 0.060 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
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'
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'
Na Na 0.0362 0.0249 '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
N1 Co1 N1 105.26(14) . 2_756
N1 Co1 N3 107.74(10) . 2_756
N1 Co1 N3 109.27(9) 2_756 2_756
N1 Co1 N3 109.27(9) . .
N1 Co1 N3 107.74(10) 2_756 .
N3 Co1 N3 116.95(14) 2_756 .
N1 Co1 Na1 159.27(7) . 2_756
N1 Co1 Na1 82.88(7) 2_756 2_756
N3 Co1 Na1 51.65(7) 2_756 2_756
N3 Co1 Na1 85.50(7) . 2_756
N1 Co1 Na1 82.88(7) . .
N1 Co1 Na1 159.27(7) 2_756 .
N3 Co1 Na1 85.50(7) 2_756 .
N3 Co1 Na1 51.65(7) . .
Na1 Co1 Na1 96.13(5) 2_756 .
N4 Na1 N2 105.83(9) 2_756 .
N4 Na1 N3 102.96(9) 2_756 .
N2 Na1 N3 89.96(9) . .
N4 Na1 C18 122.78(11) 2_756 .
N2 Na1 C18 129.37(11) . .
N3 Na1 C18 92.09(10) . .
N4 Na1 C17 144.34(10) 2_756 .
N2 Na1 C17 101.87(10) . .
N3 Na1 C17 99.03(10) . .
C18 Na1 C17 28.10(11) . .
N4 Na1 C8 129.29(9) 2_756 .
N2 Na1 C8 74.62(9) . .
N3 Na1 C8 28.01(8) . .
C18 Na1 C8 84.28(10) . .
C17 Na1 C8 79.52(9) . .
N4 Na1 C19 97.48(11) 2_756 .
N2 Na1 C19 144.83(10) . .
N3 Na1 C19 110.30(11) . .
C18 Na1 C19 27.57(11) . .
C17 Na1 C19 48.15(11) . .
C8 Na1 C19 110.11(11) . .
N4 Na1 C16 130.71(10) 2_756 .
N2 Na1 C16 90.60(9) . .
N3 Na1 C16 123.61(9) . .
C18 Na1 C16 47.95(10) . .
C17 Na1 C16 26.70(10) . .
C8 Na1 C16 99.68(9) . .
C19 Na1 C16 54.29(10) . .
N4 Na1 Co1 73.46(7) 2_756 .
N2 Na1 Co1 74.85(7) . .
N3 Na1 Co1 38.65(5) . .
C18 Na1 Co1 129.21(9) . .
C17 Na1 Co1 136.42(8) . .
C8 Na1 Co1 57.43(6) . .
C19 Na1 Co1 138.18(9) . .
C16 Na1 Co1 155.17(7) . .
C7 N1 C1 104.6(2) . .
C7 N1 Co1 132.15(19) . .
C1 N1 Co1 122.94(19) . .
C6 N2 C7 115.1(2) . .
C6 N2 Na1 121.44(19) . .
C7 N2 Na1 122.72(18) . .
C14 N3 C8 104.3(2) . .
C14 N3 Co1 125.45(18) . .
C8 N3 Co1 120.98(19) . .
C14 N3 Na1 117.37(18) . .
C8 N3 Na1 94.09(17) . .
Co1 N3 Na1 89.70(9) . .
C13 N4 C14 114.5(2) . .
C13 N4 Na1 116.88(19) . 2_756
C14 N4 Na1 125.91(19) . 2_756
C2 C1 N1 113.4(3) . .
C2 C1 H1A 123.3 . .
N1 C1 H1A 123.3 . .
C1 C2 C3 105.5(3) . .
C1 C2 H2A 127.3 . .
C3 C2 H2A 127.3 . .
C4 C3 C7 118.1(3) . .
C4 C3 C2 136.5(3) . .
C7 C3 C2 105.3(2) . .
C5 C4 C3 117.7(3) . .
C5 C4 H4A 121.2 . .
C3 C4 H4A 121.2 . .
C4 C5 C6 120.2(3) . .
C4 C5 H5A 119.9 . .
C6 C5 H5A 119.9 . .
N2 C6 C5 124.2(3) . .
N2 C6 H6A 117.9 . .
C5 C6 H6A 117.9 . .
N2 C7 N1 124.2(3) . .
N2 C7 C3 124.7(3) . .
N1 C7 C3 111.2(2) . .
C9 C8 N3 112.8(3) . .
C9 C8 Na1 125.5(2) . .
N3 C8 Na1 57.90(15) . .
C9 C8 H8A 115.5 . .
N3 C8 H8A 115.5 . .
Na1 C8 H8A 115.5 . .
C8 C9 C10 106.4(2) . .
C8 C9 H9A 126.8 . .
C10 C9 H9A 126.8 . .
C11 C10 C14 117.8(3) . .
C11 C10 C9 136.4(3) . .
C14 C10 C9 105.8(2) . .
C12 C11 C10 117.5(3) . .
C12 C11 H11A 121.2 . .
C10 C11 H11A 121.2 . .
C11 C12 C13 120.3(3) . .
C11 C12 H12A 119.8 . .
C13 C12 H12A 119.8 . .
N4 C13 C12 124.5(3) . .
N4 C13 H13A 117.7 . .
C12 C13 H13A 117.7 . .
N4 C14 N3 123.9(2) . .
N4 C14 C10 125.3(3) . .
N3 C14 C10 110.7(2) . .
C20 C15 C16 117.8(3) . .
C20 C15 C21 121.2(3) . .
C16 C15 C21 120.9(3) . .
C17 C16 C15 121.1(3) . .
C17 C16 Na1 69.05(19) . .
C15 C16 Na1 83.10(19) . .
C17 C16 H16A 119.4 . .
C15 C16 H16A 119.4 . .
Na1 C16 H16A 119.4 . .
C16 C17 C18 120.5(3) . .
C16 C17 Na1 84.2(2) . .
C18 C17 Na1 74.1(2) . .
C16 C17 H17A 119.5 . .
C18 C17 H17A 119.5 . .
Na1 C17 H17A 119.5 . .
C19 C18 C17 118.5(4) . .
C19 C18 Na1 81.5(2) . .
C17 C18 Na1 77.8(2) . .
C19 C18 H18A 120.2 . .
C17 C18 H18A 120.2 . .
Na1 C18 H18A 120.2 . .
C20 C19 C18 120.7(3) . .
C20 C19 Na1 84.5(2) . .
C18 C19 Na1 71.0(2) . .
C20 C19 H19A 119.6 . .
C18 C19 H19A 119.6 . .
Na1 C19 H19A 119.6 . .
C19 C20 C15 121.2(3) . .
C19 C20 H20A 119.4 . .
C15 C20 H20A 119.4 . .
C15 C21 H21A 109.5 . .
C15 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C15 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 1.998(2) .
Co1 N1 1.998(2) 2_756
Co1 N3 2.010(2) 2_756
Co1 N3 2.010(2) .
Co1 Na1 3.2178(13) 2_756
Co1 Na1 3.2178(13) .
Na1 N4 2.410(3) 2_756
Na1 N2 2.438(3) .
Na1 N3 2.524(3) .
Na1 C18 2.842(4) .
Na1 C17 2.889(4) .
Na1 C8 2.971(3) .
Na1 C19 2.973(4) .
Na1 C16 3.078(3) .
N1 C7 1.366(4) .
N1 C1 1.381(4) .
N2 C6 1.343(4) .
N2 C7 1.354(4) .
N3 C14 1.386(4) .
N3 C8 1.399(4) .
N4 C13 1.347(4) .
N4 C14 1.349(4) .
N4 Na1 2.410(3) 2_756
C1 C2 1.372(4) .
C1 H1A 0.9500 .
C2 C3 1.428(4) .
C2 H2A 0.9500 .
C3 C4 1.391(4) .
C3 C7 1.427(4) .
C4 C5 1.383(4) .
C4 H4A 0.9500 .
C5 C6 1.403(4) .
C5 H5A 0.9500 .
C6 H6A 0.9500 .
C8 C9 1.365(4) .
C8 H8A 1.0000 .
C9 C10 1.426(4) .
C9 H9A 0.9500 .
C10 C11 1.400(4) .
C10 C14 1.422(4) .
C11 C12 1.379(4) .
C11 H11A 0.9500 .
C12 C13 1.397(4) .
C12 H12A 0.9500 .
C13 H13A 0.9500 .
C15 C20 1.390(5) .
C15 C16 1.397(5) .
C15 C21 1.499(5) .
C16 C17 1.390(5) .
C16 H16A 1.0000 .
C17 C18 1.392(5) .
C17 H17A 1.0000 .
C18 C19 1.391(6) .
C18 H18A 1.0000 .
C19 C20 1.387(5) .
C19 H19A 1.0000 .
C20 H20A 0.9500 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
