The crystal structure of catena-poly[oktaaqua-bis(μ2-4,4′-ethene-1,2-diyldipyridine-κ2 N:N′)-(μ2-3,3′-(1-oxidodiazene-1,2-diyl)diphthalato-κ2 O:O′)dicobalt(II)] dihydrate, C28H36N4O19Co2
Feng, Xun; Chen, Nan; Zhang, Zhengtao; Yu, Jingjing; Zhang, Yiming; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 929–931; doi:10.1515/ncrs-2020-0105

data_8105334
_publ_section_title
;
 The crystal structure of
 catena-poly[oktaaqua-bis(\m2-4,4&#x2032;-ethene-1,2-diyldipyridine-\k2
 N:N&#x2032;)-(\m2-3,3&#x2032;-(1-oxidodiazene-1,2-diyl)diphthalato-\k2
 O:O&#x2032;)dicobalt(II)] dihydrate, C28H36N4O19Co2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              929
_journal_page_last               931
_journal_paper_doi               10.1515/ncrs-2020-0105
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C28 H32 Co2 N4 O17, 2(H2 O)'
_chemical_formula_sum            'C28 H36 Co2 N4 O19'
_chemical_formula_weight         850.47
_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                88.027(4)
_cell_angle_beta                 89.819(5)
_cell_angle_gamma                69.729(5)
_cell_formula_units_Z            1
_cell_length_a                   7.4890(5)
_cell_length_b                   8.8913(4)
_cell_length_c                   13.5918(7)
_cell_measurement_reflns_used    3237
_cell_measurement_temperature    290
_cell_measurement_theta_max      27.2200
_cell_measurement_theta_min      3.9330
_cell_volume                     848.44(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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_temperature      290
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.841
_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    -18.00  12.00   1.00    4.83    --  -13.80 -99.00-180.00   30
  2  \w    -72.00   0.00   1.00    4.83    --  -13.80 -57.00-120.00   72
  3  \w    -85.00 -59.00   1.00    4.83    --  -13.80-178.00  60.00   26
  4  \w    -15.00  22.00   1.00    4.83    --  -13.80 -99.00  90.00   37
  5  \w    -64.00 -39.00   1.00    4.83    --  -13.80-178.00 120.00   25
  6  \w      3.00  84.00   1.00    4.83    --   14.82  38.00  90.00   81
  7  \w    -53.00  42.00   1.00    4.83    --   14.82 -19.00 -90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0695690000
_diffrn_orient_matrix_UB_12      -0.0677447000
_diffrn_orient_matrix_UB_13      -0.0202535000
_diffrn_orient_matrix_UB_21      -0.0434855000
_diffrn_orient_matrix_UB_22      0.0226718000
_diffrn_orient_matrix_UB_23      -0.0470798000
_diffrn_orient_matrix_UB_31      0.0588562000
_diffrn_orient_matrix_UB_32      0.0462358000
_diffrn_orient_matrix_UB_33      -0.0100058000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6761
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.242
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.665
_exptl_crystal_description       block
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0368P)^2^+0.4818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3015
_reflns_number_total             3524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0105_suppl.cif
_cod_data_source_block           l56-co-bpe
_cod_database_code               8105334
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.807
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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. Others
 Fixed Sof: O1(0.5)
3.a Riding coordinates:
 O10(H10A,H10B), O6(H6A,H6B), O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14)
;