#------------------------------------------------------------------------------
#$Date: 2022-09-13 10:53:42 +0300 (Tue, 13 Sep 2022) $
#$Revision: 277794 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/57/8105759.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_8105759
loop_
_publ_author_name
'Ling-Yun, Xin'
'Zhou-Ru, Ji'
'Rong-Rong, Guo'
_publ_section_title
;
 Crystal structure of diaqua-bis(3,5-dichloroisonicotinato-κ1
 O)-bis(1,3-di(pyridin-4-yl)propane-κ1 N)cobalt(II), C38H36Cl4N6O6Co
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              495
_journal_page_last               497
_journal_paper_doi               10.1515/ncrs-2018-0491
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C19 H18 Cl2 Co0.5 N3 O3'
_chemical_formula_sum            'C19 H18 Cl2 Co0.5 N3 O3'
_chemical_formula_weight         436.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                87.947(4)
_cell_angle_beta                 82.062(4)
_cell_angle_gamma                67.258(5)
_cell_formula_units_Z            2
_cell_length_a                   9.2687(4)
_cell_length_b                   9.7747(6)
_cell_length_c                   12.0131(6)
_cell_measurement_reflns_used    4840
_cell_measurement_temperature    292.6(3)
_cell_measurement_theta_max      27.0240
_cell_measurement_theta_min      4.0590
_cell_volume                     993.95(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.6(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -20.00  26.00   1.00    4.73    --  -12.53 -99.00-150.00   46
  2  ω     35.00  86.00   1.00    4.73    --   13.55 178.00  30.00   51
  3  ω    -20.00  53.00   1.00    4.73    --   13.55 -99.00  60.00   73
  4  ω    -54.00  30.00   1.00    4.73    --   13.55 -57.00  90.00   84
  5  ω    -54.00  30.00   1.00    4.73    --   13.55 -57.00 -90.00   84
  6  ω     -3.00  81.00   1.00    4.73    --   13.55  57.00 -30.00   84
  7  ω     -5.00  83.00   1.00    4.73    --   13.55  38.00-120.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0740110000
_diffrn_orient_matrix_UB_12      -0.0302800000
_diffrn_orient_matrix_UB_13      -0.0344846000
_diffrn_orient_matrix_UB_21      0.0387028000
_diffrn_orient_matrix_UB_22      -0.0188127000
_diffrn_orient_matrix_UB_23      0.0486392000
_diffrn_orient_matrix_UB_31      -0.0061020000
_diffrn_orient_matrix_UB_32      -0.0701597000
_diffrn_orient_matrix_UB_33      0.0005549000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10406
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.494
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
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    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             449
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0397
_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)+(0.0314P)²+0.5198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3200
_reflns_number_total             3627
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2018-0491_suppl.cif
_cod_data_source_block           xly-22
_cod_original_cell_volume        993.96(10)
_cod_original_formula_sum        'C19 H18 Cl2 Co0.50 N3 O3'
_cod_database_code               8105759
_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.
;
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18)
;
_olex2_date_sample_data_collection 2017-05-02
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.419
_oxdiff_exptl_absorpt_empirical_full_min 0.437
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_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 0.0000 0.5000 1.0000 0.02412(13) Uani 1 2 d S T P . .
Cl1 Cl -0.05295(9) 0.99612(8) 0.81011(7) 0.0596(2) Uani 1 1 d . . . . .
Cl2 Cl 0.46486(11) 0.49415(10) 0.70631(8) 0.0794(3) Uani 1 1 d . . . . .
O1 O 0.2299(2) 0.7095(2) 0.94570(14) 0.0486(5) Uani 1 1 d . . . . .
O1W O -0.13683(18) 0.45474(17) 0.89209(12) 0.0339(4) Uani 1 1 d . . . . .
H1WA H -0.0810 0.4186 0.8299 0.051 Uiso 1 1 d R . . . .
H1WB H -0.1960 0.4064 0.9063 0.051 Uiso 1 1 d R . . . .
O2 O 0.08612(19) 0.61018(17) 0.86711(12) 0.0336(4) Uani 1 1 d . . . . .
N1 N 0.1956(2) 0.29802(19) 0.94660(14) 0.0282(4) Uani 1 1 d . . . . .
N2 N 0.9846(3) -0.3375(2) 0.32120(17) 0.0458(6) Uani 1 1 d . . . . .
N3 N 0.2639(5) 0.8590(4) 0.5405(2) 0.0830(10) Uani 1 1 d . . . . .
C1 C 0.1749(3) 0.1714(2) 0.93624(18) 0.0307(5) Uani 1 1 d . . . . .
H1 H 0.0739 0.1720 0.9554 0.037 Uiso 1 1 calc R . . . .
C2 C 0.2954(3) 0.0402(2) 0.89875(18) 0.0335(5) Uani 1 1 d . . . . .
H2 H 0.2750 -0.0453 0.8942 0.040 Uiso 1 1 calc R . . . .
C3 C 0.4466(3) 0.0350(2) 0.86786(17) 0.0318(5) Uani 1 1 d . . . . .
C4 C 0.4683(3) 0.1661(3) 0.87975(19) 0.0357(6) Uani 1 1 d . . . . .
H4 H 0.5680 0.1685 0.8609 0.043 Uiso 1 1 calc R . . . .
C5 C 0.3422(3) 0.2926(3) 0.91940(18) 0.0328(5) Uani 1 1 d . . . . .
H5 H 0.3601 0.3788 0.9277 0.039 Uiso 1 1 calc R . . . .
C6 C 0.5803(3) -0.1060(3) 0.82543(18) 0.0389(6) Uani 1 1 d . . . . .
H6A H 0.5477 -0.1883 0.8431 0.047 Uiso 1 1 calc R . . . .
H6B H 0.6690 -0.1203 0.8654 0.047 Uiso 1 1 calc R . . . .
C7 C 0.6354(3) -0.1104(3) 0.69923(18) 0.0371(6) Uani 1 1 d . . . . .
H7A H 0.5477 -0.0949 0.6579 0.045 Uiso 1 1 calc R . . . .
H7B H 0.6736 -0.0318 0.6806 0.045 Uiso 1 1 calc R . . . .
C8 C 0.7662(3) -0.2593(3) 0.66638(19) 0.0418(6) Uani 1 1 d . . . . .
H8A H 0.8485 -0.2759 0.7132 0.050 Uiso 1 1 calc R . . . .
H8B H 0.7242 -0.3356 0.6835 0.050 Uiso 1 1 calc R . . . .
C9 C 0.8406(3) -0.2793(2) 0.54513(18) 0.0344(6) Uani 1 1 d . . . . .
C10 C 0.7534(3) -0.2593(3) 0.4571(2) 0.0478(7) Uani 1 1 d . . . . .
H10 H 0.6438 -0.2242 0.4709 0.057 Uiso 1 1 calc R . . . .
C11 C 0.8300(4) -0.2918(3) 0.3487(2) 0.0547(8) Uani 1 1 d . . . . .
H11 H 0.7690 -0.2807 0.2912 0.066 Uiso 1 1 calc R . . . .
C12 C 1.0671(3) -0.3515(3) 0.4058(2) 0.0442(6) Uani 1 1 d . . . . .
H12 H 1.1760 -0.3808 0.3892 0.053 Uiso 1 1 calc R . . . .
C13 C 1.0005(3) -0.3248(3) 0.5169(2) 0.0393(6) Uani 1 1 d . . . . .
H13 H 1.0646 -0.3379 0.5728 0.047 Uiso 1 1 calc R . . . .
C14 C 0.1718(3) 0.6829(2) 0.86710(18) 0.0311(5) Uani 1 1 d . . . . .
C15 C 0.2054(3) 0.7462(3) 0.75318(19) 0.0365(6) Uani 1 1 d . . . . .
C16 C 0.1095(3) 0.8852(3) 0.7199(2) 0.0455(7) Uani 1 1 d . . . . .
C17 C 0.1432(5) 0.9367(4) 0.6140(3) 0.0689(10) Uani 1 1 d . . . . .
H17 H 0.0770 1.0306 0.5942 0.083 Uiso 1 1 calc R . . . .
C18 C 0.3575(5) 0.7270(4) 0.5714(3) 0.0738(11) Uani 1 1 d . . . . .
H18 H 0.4440 0.6706 0.5207 0.089 Uiso 1 1 calc R . . . .
C19 C 0.3333(4) 0.6686(3) 0.6753(2) 0.0509(7) 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'
Cl Cl 0.1484 0.1585 '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'
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
O1W Co1 O1W 180.0 . 2_567
O1W Co1 O2 90.36(6) . 2_567
O1W Co1 O2 89.64(6) . .
O1W Co1 O2 89.64(6) 2_567 2_567
O1W Co1 O2 90.36(6) 2_567 .
O1W Co1 N1 90.59(6) 2_567 2_567
O1W Co1 N1 89.41(6) 2_567 .
O1W Co1 N1 90.58(6) . .
O1W Co1 N1 89.42(6) . 2_567
O2 Co1 O2 180.00(8) . 2_567
O2 Co1 N1 91.35(6) 2_567 .
O2 Co1 N1 91.35(6) . 2_567
O2 Co1 N1 88.65(6) 2_567 2_567
O2 Co1 N1 88.65(6) . .
N1 Co1 N1 180.0 2_567 .
Co1 O1W H1WA 110.3 . .
Co1 O1W H1WB 127.9 . .
H1WA O1W H1WB 104.9 . .
C14 O2 Co1 130.50(14) . .
C1 N1 Co1 121.07(15) . .
C5 N1 Co1 122.21(14) . .
C5 N1 C1 116.70(19) . .
C11 N2 C12 115.9(2) . .
C17 N3 C18 117.2(3) . .
N1 C1 H1 118.4 . .
N1 C1 C2 123.3(2) . .
C2 C1 H1 118.4 . .
C1 C2 H2 119.9 . .
C1 C2 C3 120.2(2) . .
C3 C2 H2 119.9 . .
C2 C3 C4 116.5(2) . .
C2 C3 C6 121.4(2) . .
C4 C3 C6 122.1(2) . .
C3 C4 H4 120.0 . .
C5 C4 C3 120.0(2) . .
C5 C4 H4 120.0 . .
N1 C5 C4 123.3(2) . .
N1 C5 H5 118.3 . .
C4 C5 H5 118.3 . .
C3 C6 H6A 108.6 . .
C3 C6 H6B 108.6 . .
C3 C6 C7 114.56(19) . .
H6A C6 H6B 107.6 . .
C7 C6 H6A 108.6 . .
C7 C6 H6B 108.6 . .
C6 C7 H7A 109.8 . .
C6 C7 H7B 109.8 . .
H7A C7 H7B 108.2 . .
C8 C7 C6 109.48(19) . .
C8 C7 H7A 109.8 . .
C8 C7 H7B 109.8 . .
C7 C8 H8A 108.2 . .
C7 C8 H8B 108.2 . .
H8A C8 H8B 107.4 . .
C9 C8 C7 116.3(2) . .
C9 C8 H8A 108.2 . .
C9 C8 H8B 108.2 . .
C10 C9 C8 122.4(2) . .
C13 C9 C8 121.2(2) . .
C13 C9 C10 116.4(2) . .
C9 C10 H10 120.2 . .
C11 C10 C9 119.5(3) . .
C11 C10 H10 120.2 . .
N2 C11 C10 124.3(3) . .
N2 C11 H11 117.9 . .
C10 C11 H11 117.9 . .
N2 C12 H12 118.1 . .
N2 C12 C13 123.7(3) . .
C13 C12 H12 118.1 . .
C9 C13 C12 120.2(2) . .
C9 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
O1 C14 O2 128.8(2) . .
O1 C14 C15 117.2(2) . .
O2 C14 C15 114.02(19) . .
C16 C15 C14 122.6(2) . .
C19 C15 C14 122.3(2) . .
C19 C15 C16 115.1(2) . .
C15 C16 Cl1 120.12(19) . .
C15 C16 C17 120.4(3) . .
C17 C16 Cl1 119.5(2) . .
N3 C17 C16 123.2(3) . .
N3 C17 H17 118.4 . .
C16 C17 H17 118.4 . .
N3 C18 H18 118.4 . .
N3 C18 C19 123.2(3) . .
C19 C18 H18 118.4 . .
C15 C19 Cl2 120.1(2) . .
C18 C19 Cl2 119.0(3) . .
C18 C19 C15 120.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1W 2.1009(14) .
Co1 O1W 2.1009(14) 2_567
Co1 O2 2.1296(15) 2_567
Co1 O2 2.1296(15) .
Co1 N1 2.1441(18) 2_567
Co1 N1 2.1441(18) .
Cl1 C16 1.728(3) .
Cl2 C19 1.734(3) .
O1 C14 1.231(3) .
O1W H1WA 0.8499 .
O1W H1WB 0.8498 .
O2 C14 1.254(3) .
N1 C1 1.336(3) .
N1 C5 1.334(3) .
N2 C11 1.321(4) .
N2 C12 1.327(3) .
N3 C17 1.314(5) .
N3 C18 1.321(5) .
C1 H1 0.9300 .
C1 C2 1.374(3) .
C2 H2 0.9300 .
C2 C3 1.381(3) .
C3 C4 1.387(3) .
C3 C6 1.500(3) .
C4 H4 0.9300 .
C4 C5 1.376(3) .
C5 H5 0.9300 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.528(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C8 1.513(3) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 C9 1.508(3) .
C9 C10 1.382(3) .
C9 C13 1.368(3) .
C10 H10 0.9300 .
C10 C11 1.379(4) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C12 C13 1.380(3) .
C13 H13 0.9300 .
C14 C15 1.524(3) .
C15 C16 1.386(4) .
C15 C19 1.381(4) .
C16 C17 1.391(4) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C18 C19 1.379(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA N2 0.85 1.96 2.798(2) 170.7 2_656
O1W H1WB O1 0.85 2.13 2.738(2) 128.7 2_567
