Crystal structure of catena-poly[triaqua-(1,3-di(1H-imidazol-1-yl)benzene-κ2N:N′)-(3-nitrophthalato-κ1O)cobalt(II)] — water (2/3), C20H22N5O10.5Co
Yin, Wei-Dong; Liu, Qian-Long; Li, Gui-Lian; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 125–128; doi:10.1515/ncrs-2019-0531

data_8105036
_publ_section_title
;
 Crystal structure of
 catena-poly[triaqua-(1,3-di(1H-imidazol-1-yl)benzene-\k2N:N&#x2032;)-(3-nitrophthalato-\k1O)cobalt(II)]
 --- water (2/3), C20H22N5O10.5Co
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              125
_journal_page_last               128
_journal_paper_doi               10.1515/ncrs-2019-0531
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C20 H19 Co N5 O9, 1.5(H2 O)'
_chemical_formula_sum            'C20 H22 Co N5 O10.5'
_chemical_formula_weight         559.35
_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                81.096(3)
_cell_angle_beta                 83.110(3)
_cell_angle_gamma                69.997(4)
_cell_formula_units_Z            2
_cell_length_a                   7.9667(3)
_cell_length_b                   11.5847(4)
_cell_length_c                   13.5305(5)
_cell_measurement_reflns_used    5859
_cell_measurement_temperature    292.73(13)
_cell_measurement_theta_max      27.6330
_cell_measurement_theta_min      3.9390
_cell_volume                     1156.26(8)
_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_environment      air
_diffrn_ambient_temperature      292.73(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.840
_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    -81.00  13.00   1.00    3.14    --  -13.80 -77.00 -30.00   94
  2  \w    -31.00  53.00   1.00    3.14    --  -13.80  57.00-120.00   84
  3  \w    -20.00  25.00   1.00    3.14    --  -13.80 -99.00  90.00   45
  4  \w    -41.00  54.00   1.00    3.14    --  -13.80  77.00  90.00   95
  5  \w     -2.00  82.00   1.00    3.14    --   14.82  57.00-120.00   84
  6  \w    -54.00  34.00   1.00    3.14    --   14.82 -38.00-180.00   88
  7  \w     35.00  87.00   1.00    3.14    --   14.82 178.00  90.00   52
;
_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      0.0281481000
_diffrn_orient_matrix_UB_12      0.0367532000
_diffrn_orient_matrix_UB_13      -0.0411156000
_diffrn_orient_matrix_UB_21      0.0706947000
_diffrn_orient_matrix_UB_22      -0.0531268000
_diffrn_orient_matrix_UB_23      -0.0136377000
_diffrn_orient_matrix_UB_31      -0.0568712000
_diffrn_orient_matrix_UB_32      -0.0116807000
_diffrn_orient_matrix_UB_33      -0.0308867000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13684
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.458
_diffrn_reflns_theta_min         3.353
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63135
_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    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0430P)^2^+1.2145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4241
_reflns_number_total             4911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0531_suppl.cif
_cod_data_source_block           lgl-40
_cod_original_formula_sum        'C20 H22 Co N5 O10.50'
_cod_database_code               8105036
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.775
_reflns_odcompleteness_completeness 99.76
_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: O4W(0.5) H4WA(0.5) H4WB(0.5)
3.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O5W(H5WA,H5WB), O4W(H4WA,H4WB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
;