Crystal structure of catena-poly[diaqua-bis(μ2-3,5-di(1H-1,2,4-triazol-1-yl)benzoate-κ2 N:N′)cobalt(II))] 2.5 hydrate, C22H23CoN12O8.50
Lan, Hong-Hong; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 1003–1004; doi:10.1515/ncrs-2018-0120

data_8106377
_publ_section_title
;
 Crystal structure of
 catena-poly[diaqua-bis(\m2-3,5-di(1H-1,2,4-triazol-1-yl)benzoate-\k2
 N:N&#x2032;)cobalt(II))] 2.5 hydrate, C22H23CoN12O8.50
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1003
_journal_page_last               1004
_journal_paper_doi               10.1515/ncrs-2018-0120
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C22 H18 Co N12 O6, 2.5(H2 O)'
_chemical_formula_sum            'C22 H23 Co N12 O8.5'
_chemical_formula_weight         650.45
_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                100.824(3)
_cell_angle_beta                 99.707(3)
_cell_angle_gamma                96.642(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6549(3)
_cell_length_b                   10.6027(4)
_cell_length_c                   13.4938(4)
_cell_measurement_reflns_used    7110
_cell_measurement_temperature    288.03(10)
_cell_measurement_theta_max      27.5930
_cell_measurement_theta_min      3.8690
_cell_volume                     1321.76(8)
_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      288.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.983
_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    -39.00  55.00   1.00    2.34    --  -12.53  77.00  60.00   94
  2  \w    -13.00  81.00   1.00    2.34    --   13.55  77.00 -30.00   94
  3  \w    -13.00  81.00   1.00    2.34    --   13.55  77.00-180.00   94
  4  \w    -13.00  81.00   1.00    2.34    --   13.55  77.00  30.00   94
  5  \w    -13.00  81.00   1.00    2.34    --   13.55  77.00-150.00   94
  6  \w    -20.00  29.00   1.00    2.34    --   13.55 -99.00-120.00   49
;
_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      0.0526067000
_diffrn_orient_matrix_UB_12      0.0436440000
_diffrn_orient_matrix_UB_13      -0.0123603000
_diffrn_orient_matrix_UB_21      0.0336755000
_diffrn_orient_matrix_UB_22      0.0182003000
_diffrn_orient_matrix_UB_23      0.0526092000
_diffrn_orient_matrix_UB_31      0.0422521000
_diffrn_orient_matrix_UB_32      -0.0501286000
_diffrn_orient_matrix_UB_33      -0.0075424000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14128
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.445
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82417
_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            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.059
_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     412
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0366
_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/[\s^2^(Fo^2^)+(0.0398P)^2^+0.8481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4245
_reflns_number_total             4844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0120_suppl.cif
_cod_data_source_block           miao
_cod_original_formula_sum        'C22 H23 Co N12 O8.50'
_cod_database_code               8106377
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O2A)
3. Others
 Sof(O2A)=1-FVAR(1)
 Sof(O2)=FVAR(1)
 Fixed Sof: O9(0.5) H9A(0.5) H9B(0.5)
4.a Riding coordinates:
 O9(H9A,H9B)
4.b Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
4.c Rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C15(H15),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22)
;
_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 1.376
_oxdiff_exptl_absorpt_empirical_full_min 0.788