#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:51:45 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257541 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705240.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_7705240
loop_
_publ_author_name
'Melle, Philipp'
'Ségaud, Nathalie'
'Albrecht, Martin'
_publ_section_title
;
 Ambidentate bonding and electrochemical implications of pincer-type
 pyridylidene amide ligands in complexes of nickel, cobalt and zinc.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12662
_journal_page_last               12673
_journal_paper_doi               10.1039/d0dt02482a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C19 H17 Cl2 Co N5 O2'
_chemical_formula_sum            'C19 H17 Cl2 Co N5 O2'
_chemical_formula_weight         477.20
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-13 deposited with the CCDC.	2020-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                102.016(2)
_cell_angle_beta                 99.280(2)
_cell_angle_gamma                104.188(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9978(2)
_cell_length_b                   9.2730(2)
_cell_length_c                   14.4181(4)
_cell_measurement_reflns_used    5682
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.0170
_cell_measurement_theta_min      2.3290
_cell_volume                     988.23(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_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      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00 103.00   1.00   27.50    --   27.42  57.00   0.00  113
  2  ω    -16.00 112.00   1.00   27.50    --   27.42  77.00 -90.00  128
  3  ω    -16.00 112.00   1.00   27.50    --   27.42  77.00  30.00  128
  4  ω    -10.00 103.00   1.00   27.50    --   27.42  57.00-180.00  113
  5  ω     35.00 122.00   1.00   27.50    --   27.42 178.00 -90.00   87
  6  ω     35.00 122.00   1.00   27.50    --   27.42 178.00-180.00   87
  7  ω   -108.00 -55.00   1.00   27.50    --  -23.50-153.00-144.00   53
  8  ω    -54.00  83.00   1.00   27.50    --   27.42 -38.00  30.00  137
  9  ω     35.00 122.00   1.00   27.50    --   27.42 178.00 -30.00   87
 10  ω    -16.00  63.00   1.00   27.50    --   27.42  77.00 120.00   79
 11  ω    -49.00  65.00   1.00   27.50    --   27.42 -57.00 -90.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0587525000
_diffrn_orient_matrix_UB_12      0.0269970000
_diffrn_orient_matrix_UB_13      -0.0287144000
_diffrn_orient_matrix_UB_21      -0.0685854000
_diffrn_orient_matrix_UB_22      -0.0347918000
_diffrn_orient_matrix_UB_23      -0.0425092000
_diffrn_orient_matrix_UB_31      -0.0255688000
_diffrn_orient_matrix_UB_32      0.0687950000
_diffrn_orient_matrix_UB_33      0.0056342000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16903
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.103
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       prism
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0303P)²+0.3672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3596
_reflns_number_total             4480
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02482a2.cif
_cod_data_source_block           19ma035_PM305
_cod_depositor_comments
'Adding full bibliography for 7705237--7705245.cif.'
_cod_original_cell_volume        988.23(4)
_cod_database_code               7705240
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C19H17Cl2Co1N5O2
_chemical_oxdiff_usercomment     PM305
_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   0.944
_shelx_estimated_absorpt_t_min   0.845
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H22A,H22B,H22C} of C22
 At 1.5 times of:
  {H29A,H29B,H29C} of C29
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C17(H17), C24(H24), C7(H7), C27(H27), C18(H18), C25(H25),
 C20(H20), C19(H19), C26(H26)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C22(H22A,H22B,H22C)
;
_olex2_date_sample_data_collection 2019-03-01
_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 1.647
_oxdiff_exptl_absorpt_empirical_full_min 0.750
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 0.23093(4) 0.26103(3) 0.25612(2) 0.02743(9) Uani 1 1 d . . . . .
Cl2 Cl 0.15728(7) 0.03171(6) 0.14444(4) 0.03306(13) Uani 1 1 d . . . . .
Cl3 Cl 0.01686(7) 0.36517(6) 0.29423(4) 0.03629(14) Uani 1 1 d . . . . .
O14 O 0.29100(19) 0.17872(16) 0.38857(10) 0.0295(3) Uani 1 1 d . . . . .
O11 O 0.30632(19) 0.40747(16) 0.15737(10) 0.0306(3) Uani 1 1 d . . . . .
N4 N 0.4804(2) 0.39093(18) 0.32236(12) 0.0235(4) Uani 1 1 d . . . . .
N15 N 0.5195(2) 0.23556(19) 0.52674(12) 0.0261(4) Uani 1 1 d . . . . .
N21 N 0.5452(2) 0.12546(18) 0.65388(12) 0.0265(4) Uani 1 1 d . . . . .
N28 N 0.5482(2) 0.74617(19) 0.03403(12) 0.0280(4) Uani 1 1 d . . . . .
N12 N 0.5331(2) 0.61886(19) 0.15383(12) 0.0272(4) Uani 1 1 d . . . . .
C9 C 0.5558(3) 0.3753(2) 0.40819(14) 0.0242(4) Uani 1 1 d . . . . .
C23 C 0.4425(3) 0.6579(2) 0.07979(15) 0.0265(4) Uani 1 1 d . . . . .
C13 C 0.4409(3) 0.2514(2) 0.44223(15) 0.0254(4) Uani 1 1 d . . . . .
C5 C 0.5649(3) 0.4988(2) 0.28308(14) 0.0240(4) Uani 1 1 d . . . . .
C16 C 0.4365(3) 0.1364(2) 0.57284(14) 0.0260(4) Uani 1 1 d . . . . .
C10 C 0.4547(3) 0.5056(2) 0.18971(15) 0.0254(4) Uani 1 1 d . . . . .
C6 C 0.7332(3) 0.5930(2) 0.32832(15) 0.0281(4) Uani 1 1 d . . . . .
H6 H 0.7926 0.6651 0.2998 0.034 Uiso 1 1 calc R . . . .
C8 C 0.7227(3) 0.4689(2) 0.45831(15) 0.0276(4) Uani 1 1 d . . . . .
H8 H 0.7739 0.4586 0.5184 0.033 Uiso 1 1 calc R . . . .
C17 C 0.2582(3) 0.0488(2) 0.55235(16) 0.0312(5) Uani 1 1 d . . . . .
H17 H 0.1803 0.0525 0.4981 0.037 Uiso 1 1 calc R . . . .
C24 C 0.2589(3) 0.6298(2) 0.04950(16) 0.0335(5) Uani 1 1 d . . . . .
H24 H 0.1833 0.5706 0.0790 0.040 Uiso 1 1 calc R . . . .
C7 C 0.8116(3) 0.5776(2) 0.41733(16) 0.0309(5) Uani 1 1 d . . . . .
H7 H 0.9244 0.6407 0.4495 0.037 Uiso 1 1 calc R . . . .
C27 C 0.4787(3) 0.8016(2) -0.03846(16) 0.0351(5) Uani 1 1 d . . . . .
H27 H 0.5544 0.8596 -0.0685 0.042 Uiso 1 1 calc R . . . .
C18 C 0.1967(3) -0.0419(2) 0.61047(16) 0.0339(5) Uani 1 1 d . . . . .
H18 H 0.0780 -0.0982 0.5961 0.041 Uiso 1 1 calc R . . . .
C29 C 0.7414(3) 0.7852(3) 0.06540(17) 0.0356(5) Uani 1 1 d . . . . .
H29A H 0.7785 0.8463 0.1316 0.053 Uiso 1 1 calc GR . . . .
H29B H 0.7960 0.8426 0.0245 0.053 Uiso 1 1 calc GR . . . .
H29C H 0.7760 0.6924 0.0606 0.053 Uiso 1 1 calc GR . . . .
C25 C 0.1894(3) 0.6878(3) -0.02249(18) 0.0399(6) Uani 1 1 d . . . . .
H25 H 0.0676 0.6694 -0.0410 0.048 Uiso 1 1 calc R . . . .
C20 C 0.4843(3) 0.0349(2) 0.71102(16) 0.0329(5) Uani 1 1 d . . . . .
H20 H 0.5623 0.0306 0.7650 0.039 Uiso 1 1 calc R . . . .
C22 C 0.7339(3) 0.2144(3) 0.67990(16) 0.0345(5) Uani 1 1 d . . . . .
H22A H 0.7862 0.1912 0.6253 0.041 Uiso 1 1 calc GR . . . .
H22B H 0.7939 0.1873 0.7340 0.041 Uiso 1 1 calc GR . . . .
H22C H 0.7444 0.3225 0.6974 0.041 Uiso 1 1 calc GR . . . .
C19 C 0.3127(3) -0.0495(2) 0.69123(16) 0.0346(5) Uani 1 1 d . . . . .
H19 H 0.2729 -0.1114 0.7309 0.041 Uiso 1 1 calc R . . . .
C26 C 0.3020(3) 0.7745(3) -0.06797(17) 0.0394(6) Uani 1 1 d . . . . .
H26 H 0.2563 0.8131 -0.1178 0.047 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 0.0033 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
_geom_angle_publ_flag
Cl3 Co1 Cl2 119.54(2) . . ?
O14 Co1 Cl2 97.98(4) . . ?
O14 Co1 Cl3 98.69(4) . . ?
O11 Co1 Cl2 96.80(4) . . ?
O11 Co1 Cl3 94.51(4) . . ?
O11 Co1 O14 151.97(5) . . ?
N4 Co1 Cl2 125.11(5) . . ?
N4 Co1 Cl3 115.28(5) . . ?
N4 Co1 O14 76.10(6) . . ?
N4 Co1 O11 75.91(6) . . ?
C13 O14 Co1 113.40(13) . . ?
C10 O11 Co1 113.85(12) . . ?
C9 N4 Co1 119.49(13) . . ?
C9 N4 C5 120.66(18) . . ?
C5 N4 Co1 119.72(13) . . ?
C13 N15 C16 122.29(18) . . ?
C16 N21 C22 119.43(17) . . ?
C20 N21 C16 122.02(18) . . ?
C20 N21 C22 118.54(17) . . ?
C23 N28 C29 119.54(17) . . ?
C27 N28 C23 121.69(18) . . ?
C27 N28 C29 118.75(18) . . ?
C10 N12 C23 121.00(18) . . ?
N4 C9 C13 113.48(17) . . ?
N4 C9 C8 120.96(18) . . ?
C8 C9 C13 125.55(18) . . ?
N28 C23 C24 116.98(18) . . ?
N12 C23 N28 114.09(18) . . ?
N12 C23 C24 128.74(19) . . ?
O14 C13 N15 130.02(19) . . ?
O14 C13 C9 117.42(17) . . ?
N15 C13 C9 112.56(17) . . ?
N4 C5 C10 112.97(17) . . ?
N4 C5 C6 121.11(19) . . ?
C6 C5 C10 125.90(18) . . ?
N15 C16 N21 113.50(18) . . ?
N15 C16 C17 130.01(19) . . ?
N21 C16 C17 116.46(18) . . ?
O11 C10 N12 129.52(19) . . ?
O11 C10 C5 117.24(17) . . ?
N12 C10 C5 113.24(18) . . ?
C5 C6 H6 120.8 . . ?
C5 C6 C7 118.46(19) . . ?
C7 C6 H6 120.8 . . ?
C9 C8 H8 120.7 . . ?
C7 C8 C9 118.64(19) . . ?
C7 C8 H8 120.7 . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.5(2) . . ?
C18 C17 H17 119.3 . . ?
C23 C24 H24 119.4 . . ?
C25 C24 C23 121.2(2) . . ?
C25 C24 H24 119.4 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.14(19) . . ?
C8 C7 H7 119.9 . . ?
N28 C27 H27 119.3 . . ?
C26 C27 N28 121.5(2) . . ?
C26 C27 H27 119.3 . . ?
C17 C18 H18 120.2 . . ?
C17 C18 C19 119.7(2) . . ?
C19 C18 H18 120.2 . . ?
N28 C29 H29A 109.5 . . ?
N28 C29 H29B 109.5 . . ?
N28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 119.7(2) . . ?
C26 C25 H25 120.2 . . ?
N21 C20 H20 119.3 . . ?
C19 C20 N21 121.5(2) . . ?
C19 C20 H20 119.3 . . ?
N21 C22 H22A 109.5 . . ?
N21 C22 H22B 109.5 . . ?
N21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C19 H19 120.5 . . ?
C20 C19 C18 118.9(2) . . ?
C20 C19 H19 120.5 . . ?
C27 C26 C25 118.9(2) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
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 Cl2 2.2619(6) . ?
Co1 Cl3 2.2491(6) . ?
Co1 O14 2.2250(14) . ?
Co1 O11 2.2171(14) . ?
Co1 N4 2.0181(16) . ?
O14 C13 1.256(2) . ?
O11 C10 1.253(2) . ?
N4 C9 1.339(2) . ?
N4 C5 1.343(2) . ?
N15 C13 1.332(2) . ?
N15 C16 1.351(3) . ?
N21 C16 1.377(2) . ?
N21 C20 1.356(3) . ?
N21 C22 1.476(3) . ?
N28 C23 1.373(2) . ?
N28 C27 1.357(3) . ?
N28 C29 1.468(3) . ?
N12 C23 1.355(3) . ?
N12 C10 1.331(3) . ?
C9 C13 1.506(3) . ?
C9 C8 1.385(3) . ?
C23 C24 1.405(3) . ?
C5 C10 1.508(3) . ?
C5 C6 1.380(3) . ?
C16 C17 1.406(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.386(3) . ?
C8 H8 0.9300 . ?
C8 C7 1.380(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.369(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.367(3) . ?
C7 H7 0.9300 . ?
C27 H27 0.9300 . ?
C27 C26 1.353(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.392(3) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C25 H25 0.9300 . ?
C25 C26 1.394(3) . ?
C20 H20 0.9300 . ?
C20 C19 1.354(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C19 H19 0.9300 . ?
C26 H26 0.9300 . ?
