#------------------------------------------------------------------------------
#$Date: 2021-07-15 12:00:35 +0300 (Thu, 15 Jul 2021) $
#$Revision: 267553 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/41/1564165.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_1564165
loop_
_publ_author_name
'Wang, Min-Min'
'Wang, Chun'
'Wang, Miao'
'Wang, Jin'
'Zhu, Jin-Li'
'Hu, Lan-Ping'
'Sun, Tong-Ming'
'Tang, Yan-Feng'
_publ_section_title
;
 Synthesis and magnetic property of a cobalt complex constructed by a
 linear Co--NNN--Co unit
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119804
_journal_paper_doi               10.1016/j.ica.2020.119804
_journal_volume                  511
_journal_year                    2020
_chemical_formula_moiety         'C64 H64 Co2 N19 O2'
_chemical_formula_sum            'C67 H90 Cl3 Co2 N19 O10'
_chemical_formula_weight         1545.78
_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_Hall           '-P 4 2n'
_space_group_name_H-M_alt        'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0083(6)
_cell_length_b                   16.0083(6)
_cell_length_c                   29.6119(11)
_cell_measurement_reflns_used    1091
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      50.6670
_cell_measurement_theta_min      3.1240
_cell_volume                     7588.5(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   14.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3979   57.0000   60.0000 89

#__ type_ start__ end____ width___ exp.time_
  2 omega   70.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   61.0000  -60.0000 88

#__ type_ start__ end____ width___ exp.time_
  3 omega   86.00  160.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  111.0000 -120.0000 74

#__ type_ start__ end____ width___ exp.time_
  4 omega   69.00  151.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   61.0000  -30.0000 82

#__ type_ start__ end____ width___ exp.time_
  5 omega   32.00   83.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -94.0000    0.0000 51
;
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0052589000
_diffrn_orient_matrix_UB_12      -0.0175590000
_diffrn_orient_matrix_UB_13      -0.0511011000
_diffrn_orient_matrix_UB_21      0.0862209000
_diffrn_orient_matrix_UB_22      0.0407813000
_diffrn_orient_matrix_UB_23      -0.0066961000
_diffrn_orient_matrix_UB_31      0.0423648000
_diffrn_orient_matrix_UB_32      -0.0853634000
_diffrn_orient_matrix_UB_33      0.0072574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12749
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        59.999
_diffrn_reflns_theta_max         59.999
_diffrn_reflns_theta_min         3.138
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.951
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1123P)²+4.3702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2172
_refine_ls_wR_factor_ref         0.2487
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1593
_reflns_number_total             2875
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-511-119804.cif
_cod_data_source_block           Co2
_cod_original_cell_volume        7588.5(6)
_cod_database_code               1564165
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.441
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N5) = Uanis(N4) = Uanis(N3)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C9(H9A,H9B,H9C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.500000 0.500000 0.63092(6) 0.0611(5) Uani 1 4 d S T P . .
Co2 Co 0.500000 0.500000 0.84724(6) 0.0787(7) Uani 1 4 d S T P . .
O1 O 0.500000 0.500000 0.5564(3) 0.091(3) Uani 1 4 d S T P . .
O2 O 0.500000 0.500000 0.9261(4) 0.137(5) Uani 1 4 d S T P . .
N1 N 0.4429(3) 0.3803(3) 0.62728(16) 0.0635(12) Uani 1 1 d . . . . .
N2 N 0.4249(4) 0.2483(4) 0.60688(18) 0.0824(16) Uani 1 1 d . . . . .
N3 N 0.500000 0.500000 0.7023(3) 0.0877(19) Uani 1 4 d S T P . .
N4 N 0.500000 0.500000 0.7400(3) 0.0877(19) Uani 1 4 d S T P . .
N5 N 0.500000 0.500000 0.7774(3) 0.0877(19) Uani 1 4 d S T P . .
N6 N 0.6288(4) 0.5322(4) 0.85333(19) 0.0830(16) Uani 1 1 d . . . . .
N7 N 0.7414(5) 0.5861(4) 0.8852(2) 0.1020(19) Uani 1 1 d . . . . .
C1 C 0.4700(4) 0.3192(5) 0.6016(2) 0.0767(19) Uani 1 1 d . . . . .
H1 H 0.516118 0.324162 0.581611 0.092 Uiso 1 1 calc R . . . .
C2 C 0.4397(6) 0.1660(5) 0.5831(4) 0.127(3) Uani 1 1 d . . . . .
H2A H 0.453582 0.123018 0.605445 0.191 Uiso 1 1 calc GR . . . .
H2B H 0.486130 0.172067 0.561765 0.191 Uiso 1 1 calc GR . . . .
H2C H 0.389140 0.149641 0.566717 0.191 Uiso 1 1 calc GR . . . .
C3 C 0.3631(4) 0.2641(4) 0.6383(2) 0.0747(18) Uani 1 1 d . . . . .
C4 C 0.3005(5) 0.2152(5) 0.6557(3) 0.093(2) Uani 1 1 d . . . . .
H4 H 0.292847 0.158816 0.646598 0.112 Uiso 1 1 calc R . . . .
C5 C 0.2504(5) 0.2517(5) 0.6866(3) 0.095(2) Uani 1 1 d . . . . .
H5 H 0.206405 0.219816 0.699450 0.114 Uiso 1 1 calc R . . . .
C6 C 0.2607(5) 0.3343(5) 0.7003(3) 0.096(2) Uani 1 1 d . . . . .
H6 H 0.223371 0.357167 0.721927 0.116 Uiso 1 1 calc R . . . .
C7 C 0.3242(4) 0.3839(4) 0.6830(2) 0.0746(18) Uani 1 1 d . . . . .
H7 H 0.331574 0.440188 0.692391 0.090 Uiso 1 1 calc R . . . .
C8 C 0.3760(4) 0.3473(4) 0.6513(2) 0.0661(16) Uani 1 1 d . . . . .
C9 C 0.7949(6) 0.6313(6) 0.9182(4) 0.135(3) Uani 1 1 d . . . . .
H9A H 0.838079 0.593460 0.929720 0.203 Uiso 1 1 calc GR . . . .
H9B H 0.760457 0.651181 0.943363 0.203 Uiso 1 1 calc GR . . . .
H9C H 0.821483 0.679078 0.903302 0.203 Uiso 1 1 calc GR . . . .
C10 C 0.6594(5) 0.5763(6) 0.8870(3) 0.098(2) Uani 1 1 d . . . . .
H10 H 0.625693 0.598961 0.910375 0.118 Uiso 1 1 calc R . . . .
C11 C 0.7691(6) 0.5442(5) 0.8470(3) 0.098(2) Uani 1 1 d . . . . .
C12 C 0.8474(6) 0.5343(5) 0.8275(4) 0.118(3) Uani 1 1 d . . . . .
H12 H 0.896005 0.555367 0.841950 0.142 Uiso 1 1 calc R . . . .
C13 C 0.8525(7) 0.4953(6) 0.7887(5) 0.141(4) Uani 1 1 d . . . . .
H13 H 0.905011 0.491775 0.773931 0.169 Uiso 1 1 calc R . . . .
C14 C 0.7818(8) 0.4582(6) 0.7684(3) 0.125(3) Uani 1 1 d . . . . .
H14 H 0.788701 0.426590 0.741477 0.150 Uiso 1 1 calc R . . . .
C15 C 0.7028(6) 0.4667(5) 0.7867(3) 0.093(2) Uani 1 1 d . . . . .
H15 H 0.654901 0.443306 0.772495 0.111 Uiso 1 1 calc R . . . .
C16 C 0.6970(5) 0.5107(4) 0.8264(2) 0.0783(18) 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 0.0181 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'
Co Co -2.3653 3.6143 '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'
O O 0.0492 0.0322 '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'
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 O1 87.09(13) . .
N1 Co1 O1 87.09(13) 4_565 .
N1 Co1 O1 87.09(13) 2_665 .
N1 Co1 O1 87.09(13) 3_655 .
N1 Co1 N1 174.2(3) 4_565 3_655
N1 Co1 N1 174.2(3) . 2_665
N1 Co1 N1 89.852(15) . 4_565
N1 Co1 N1 89.853(14) 2_665 4_565
N1 Co1 N1 89.853(15) 2_665 3_655
N1 Co1 N1 89.854(14) . 3_655
N3 Co1 O1 180.0 . .
N3 Co1 N1 92.91(14) . 2_665
N3 Co1 N1 92.91(14) . 4_565
N3 Co1 N1 92.91(14) . 3_655
N3 Co1 N1 92.91(14) . .
N5 Co2 O2 180.0 . .
N5 Co2 N6 94.85(16) . 2_665
N5 Co2 N6 94.85(16) . 3_655
N5 Co2 N6 94.85(16) . .
N5 Co2 N6 94.85(16) . 4_565
N6 Co2 O2 85.15(16) . .
N6 Co2 O2 85.15(16) 3_655 .
N6 Co2 O2 85.15(16) 2_665 .
N6 Co2 O2 85.15(16) 4_565 .
N6 Co2 N6 170.3(3) 3_655 4_565
N6 Co2 N6 89.59(3) . 3_655
N6 Co2 N6 89.59(3) 2_665 3_655
N6 Co2 N6 170.3(3) . 2_665
N6 Co2 N6 89.59(3) . 4_565
N6 Co2 N6 89.59(3) 2_665 4_565
C1 N1 Co1 124.0(4) . .
C1 N1 C8 105.6(5) . .
C8 N1 Co1 130.3(4) . .
C1 N2 C2 126.3(7) . .
C1 N2 C3 107.8(5) . .
C3 N2 C2 125.9(7) . .
N4 N3 Co1 180.0 . .
N5 N4 N3 180.0 . .
N4 N5 Co2 180.0 . .
C10 N6 Co2 123.6(5) . .
C10 N6 C16 105.9(6) . .
C16 N6 Co2 130.5(5) . .
C10 N7 C9 127.1(8) . .
C10 N7 C11 107.0(7) . .
C11 N7 C9 126.0(8) . .
N1 C1 N2 112.4(6) . .
N1 C1 H1 123.8 . .
N2 C1 H1 123.8 . .
N2 C2 H2A 109.5 . .
N2 C2 H2B 109.5 . .
N2 C2 H2C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N2 C3 C8 104.7(6) . .
C4 C3 N2 132.2(7) . .
C4 C3 C8 123.1(7) . .
C3 C4 H4 121.9 . .
C5 C4 C3 116.2(7) . .
C5 C4 H4 121.9 . .
C4 C5 H5 118.7 . .
C4 C5 C6 122.6(7) . .
C6 C5 H5 118.7 . .
C5 C6 H6 119.2 . .
C7 C6 C5 121.5(7) . .
C7 C6 H6 119.2 . .
C6 C7 H7 121.7 . .
C8 C7 C6 116.5(7) . .
C8 C7 H7 121.7 . .
N1 C8 C3 109.4(6) . .
C7 C8 N1 130.5(6) . .
C7 C8 C3 120.1(6) . .
N7 C9 H9A 109.5 . .
N7 C9 H9B 109.5 . .
N7 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N6 C10 N7 113.7(7) . .
N6 C10 H10 123.1 . .
N7 C10 H10 123.1 . .
N7 C11 C12 133.0(9) . .
N7 C11 C16 106.0(7) . .
C12 C11 C16 121.0(8) . .
C11 C12 H12 120.8 . .
C13 C12 C11 118.3(10) . .
C13 C12 H12 120.8 . .
C12 C13 H13 119.2 . .
C12 C13 C14 121.6(9) . .
C14 C13 H13 119.2 . .
C13 C14 H14 119.2 . .
C15 C14 C13 121.6(9) . .
C15 C14 H14 119.2 . .
C14 C15 H15 121.7 . .
C16 C15 C14 116.5(9) . .
C16 C15 H15 121.7 . .
N6 C16 C11 107.5(6) . .
C15 C16 N6 131.8(7) . .
C15 C16 C11 120.7(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.208(8) .
Co1 N1 2.126(5) 3_655
Co1 N1 2.126(5) .
Co1 N1 2.126(5) 4_565
Co1 N1 2.126(5) 2_665
Co1 N3 2.113(10) .
Co2 O2 2.335(11) .
Co2 N5 2.067(10) .
Co2 N6 2.133(6) 3_655
Co2 N6 2.133(6) 4_565
Co2 N6 2.133(6) 2_665
Co2 N6 2.133(6) .
N1 C1 1.312(8) .
N1 C8 1.391(8) .
N2 C1 1.354(9) .
N2 C2 1.513(9) .
N2 C3 1.381(9) .
N3 N4 1.117(12) .
N4 N5 1.109(13) .
N6 C10 1.316(9) .
N6 C16 1.396(9) .
N7 C9 1.488(11) .
N7 C10 1.324(10) .
N7 C11 1.388(10) .
C1 H1 0.9500 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.373(10) .
C3 C8 1.401(9) .
C4 H4 0.9500 .
C4 C5 1.348(10) .
C5 H5 0.9500 .
C5 C6 1.393(11) .
C6 H6 0.9500 .
C6 C7 1.388(10) .
C7 H7 0.9500 .
C7 C8 1.382(9) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10 0.9500 .
C11 C12 1.388(12) .
C11 C16 1.410(11) .
C12 H12 0.9500 .
C12 C13 1.310(15) .
C13 H13 0.9500 .
C13 C14 1.413(15) .
C14 H14 0.9500 .
C14 C15 1.383(12) .
C15 H15 0.9500 .
C15 C16 1.375(10) .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.116 -0.771 0.500 904.0 284.2 3Cl+3CH3OH+5H2O
2 -0.519 -0.860 0.000 904.0 284.2 ?
3 0.000 0.350 0.177 9.9 0.0 ?
4 0.000 0.350 0.823 9.9 0.0 ?
5 0.000 0.650 0.177 9.9 0.0 ?
6 0.000 0.650 0.823 9.9 0.0 ?
7 0.150 0.500 0.323 9.9 0.0 ?
8 0.150 0.500 0.677 9.9 0.0 ?
9 0.350 0.000 0.177 9.9 0.0 ?
10 0.350 0.000 0.823 9.9 0.0 ?
11 0.500 0.150 0.323 9.9 0.0 ?
12 0.500 0.150 0.677 9.9 0.0 ?
13 0.500 0.850 0.323 9.9 0.0 ?
14 0.500 0.850 0.677 9.9 0.0 ?
15 0.650 0.000 0.177 9.9 0.0 ?
16 0.650 0.000 0.823 9.9 0.0 ?
17 0.850 0.500 0.323 9.9 0.0 ?
18 0.850 0.500 0.677 9.9 0.0 ?
