Crystal structure of 2-chloro-6-formylphenolato-κ2O,O′-(6,6′-(((2,2-dimethylpropane-1,3-diyl)bis(azaneylylidene))bis(methaneylylidene))bis(2-chlorophenolato)κ4 N,N,O,O′)cobalt(III), C26H22Cl3CoN2O4
Lan, Qiaoling; Huang, Meifen; Xu, Jiajun; Wu, Qiong; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1109–1111; doi:10.1515/ncrs-2022-0306

data_8107306
_publ_section_title
;
 Crystal structure of
 2-chloro-6-formylphenolato-\k2O,O&#x2032;-(6,6&#x2032;-(((2,2-dimethylpropane-1,3-diyl)bis(azaneylylidene))bis(methaneylylidene))bis(2-chlorophenolato)\k4
 N,N,O,O&#x2032;)cobalt(III), C26H22Cl3CoN2O4
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1109
_journal_page_last               1111
_journal_paper_doi               10.1515/ncrs-2022-0306
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C26 H22 Cl3 Co N2 O4'
_chemical_formula_sum            'C26 H22 Cl3 Co N2 O4'
_chemical_formula_weight         591.73
_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   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                83.900(3)
_cell_angle_beta                 66.911(4)
_cell_angle_gamma                64.232(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1835(5)
_cell_length_b                   11.6782(5)
_cell_length_c                   11.9295(5)
_cell_measurement_reflns_used    6820
_cell_measurement_temperature    213.00(10)
_cell_measurement_theta_max      75.7760
_cell_measurement_theta_min      4.0160
_cell_volume                     1286.83(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      213.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     93.00 118.00   1.00    0.10    --   48.46 163.00  61.00   25
  2  \w     70.00 118.00   1.00    0.60    --  105.98 163.00  61.00   48
  3  \w    106.00 162.00   1.00    0.60    --  105.98 116.00 -87.00   56
  4  \w     93.00 173.00   1.00    0.60    --  105.98  15.00 -90.00   80
  5  \w     50.00  82.00   1.00    0.60    --  105.98 -94.00  30.00   32
  6  \w     45.00  71.00   1.00    0.60    --  105.98-125.00  90.00   26
  7  \w     43.00  73.00   1.00    0.60    --  105.98-125.00 120.00   30
  8  \w     78.00 112.00   1.00    0.60    --  105.98-125.00 120.00   34
  9  \w     76.00 112.00   1.00    0.60    --  105.98-125.00  90.00   36
 10  \w     98.00 137.00   1.00    0.60    --  105.98-163.00  35.00   39
 11  \w     71.00  97.00   1.00    0.10    --   48.46-163.00  35.00   26
 12  \w     74.00 104.00   1.00    0.60    --  105.98-116.00-175.00   30
 13  \w     35.00 108.00   1.00    0.60    --  105.98-125.00-120.00   73
 14  \w     49.00 112.00   1.00    0.60    --  105.98-125.00 -90.00   63
 15  \w     35.00  79.00   1.00    0.10    --   48.46-116.00-175.00   44
 16  \w     35.00  71.00   1.00    0.60    --  105.98 -61.00 -30.00   36
 17  \w     39.00  68.00   1.00    0.60    --  105.98 -61.00  60.00   29
 18  \w     36.00  68.00   1.00    0.60    --  105.98 -61.00  90.00   32
 19  \w    -26.00  16.00   1.00    0.10    --  -48.46  19.00-180.00   42
 20  \w    -23.00  27.00   1.00    0.10    --  -48.46  19.00-120.00   50
 21  \w    -22.00  17.00   1.00    0.10    --  -48.46  19.00  30.00   39
 22  \w    -26.00  27.00   1.00    0.10    --  -48.46  19.00 120.00   53
 23  \w    -48.00 -21.00   1.00    0.60    --  -91.75  45.00  30.00   27
 24  \w    -60.00  -8.00   1.00    0.10    --  -48.46 116.00 -87.00   52
 25  \w    -81.00 -27.00   1.00    0.60    --  -91.75 116.00 -87.00   54
 26  \w    -96.00 -71.00   1.00    0.10    --  -48.46 163.00  61.00   25
 27  \w    -67.00 -33.00   1.00    0.60    --  -91.75 163.00  61.00   34
 28  \w   -161.00 -78.00   1.00    0.60    --  -91.75 -15.00  30.00   83
 29  \w   -117.00 -79.00   1.00    0.60    --  -91.75 -45.00-120.00   38
 30  \w   -163.00-121.00   1.00    0.60    --  -91.75 -45.00-120.00   42
 31  \w   -162.00 -76.00   1.00    0.60    --  -91.75 -77.00-150.00   86
 32  \w    -80.00 -50.00   1.00    0.10    --  -48.46-163.00  35.00   30
 33  \w   -139.00-107.00   1.00    0.60    --  -91.75-163.00  35.00   32
 34  \w   -161.00 -83.00   1.00    0.60    --  -91.75 -94.00 150.00   78
 35  \w    -73.00 -48.00   1.00    0.60    --  -91.75-163.00  35.00   25
 36  \w   -120.00 -75.00   1.00    0.10    --  -48.46-125.00-120.00   45
 37  \w   -145.00-120.00   1.00    0.60    --  -91.75-116.00-175.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0463139000
_diffrn_orient_matrix_UB_12      0.0945273000
_diffrn_orient_matrix_UB_13      -0.0916685000
_diffrn_orient_matrix_UB_21      0.1414101000
_diffrn_orient_matrix_UB_22      -0.0826123000
_diffrn_orient_matrix_UB_23      -0.1047709000
_diffrn_orient_matrix_UB_31      -0.0732215000
_diffrn_orient_matrix_UB_32      -0.0763360000
_diffrn_orient_matrix_UB_33      -0.0211411000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14183
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.019
_diffrn_reflns_theta_min         4.041
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0375
_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/[\s^2^(Fo^2^)+(0.0388P)^2^+0.4164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4515
_reflns_number_total             4954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0306_suppl.cif
_cod_data_source_block           lql1
_cod_database_code               8107306
_shelx_estimated_absorpt_t_max   0.347
_shelx_estimated_absorpt_t_min   0.313
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C15(H15), C16(H16), C17(H17),
 C20(H20), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              92242
_shelx_hkl_checksum              55115
_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 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.783