Crystal structure of diaqua-bis(3,5-dichloroisonicotinato-κ1 O)-bis(1,3-di(pyridin-4-yl)propane-κ1 N)cobalt(II), C38H36Cl4N6O6Co
Ling-Yun, Xin; Zhou-Ru, Ji; Rong-Rong, Guo; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 495–497; doi:10.1515/ncrs-2018-0491

data_8105759
_publ_section_title
;
 Crystal structure of diaqua-bis(3,5-dichloroisonicotinato-\k1
 O)-bis(1,3-di(pyridin-4-yl)propane-\k1 N)cobalt(II), C38H36Cl4N6O6Co
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur 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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -20.00  26.00   1.00    4.73    --  -12.53 -99.00-150.00   46
  2  \w     35.00  86.00   1.00    4.73    --   13.55 178.00  30.00   51
  3  \w    -20.00  53.00   1.00    4.73    --   13.55 -99.00  60.00   73
  4  \w    -54.00  30.00   1.00    4.73    --   13.55 -57.00  90.00   84
  5  \w    -54.00  30.00   1.00    4.73    --   13.55 -57.00 -90.00   84
  6  \w     -3.00  81.00   1.00    4.73    --   13.55  57.00 -30.00   84
  7  \w     -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       '\w 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/[\s^2^(Fo^2^)+(0.0314P)^2^+0.5198P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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