Crystal structure of poly[diaqua-(μ2-5-isopropoxyisophthalato-κ2 O:O′)-(μ2-(1,3-bis(3,5-di(1H-imidazol-1-yl)pyridine))-κ2 N:N′)cobalt(II)] monohydrate, C22H25N5O8Co
Zhao, Ying; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1023–1025; doi:10.1515/ncrs-2020-0135

data_8105367
_publ_section_title
;
 Crystal structure of poly[diaqua-(\m2-5-isopropoxyisophthalato-\k2
 O:O&#x2032;)-(\m2-(1,3-bis(3,5-di(1H-imidazol-1-yl)pyridine))-\k2
 N:N&#x2032;)cobalt(II)] monohydrate, C22H25N5O8Co
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1023
_journal_page_last               1025
_journal_paper_doi               10.1515/ncrs-2020-0135
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C22 H23 Co N5 O7, H2 O'
_chemical_formula_sum            'C22 H25 Co N5 O8'
_chemical_formula_weight         546.406
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 95.133(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8425(3)
_cell_length_b                   18.1807(10)
_cell_length_c                   17.0436(7)
_cell_measurement_reflns_used    2703
_cell_measurement_temperature    293.18(10)
_cell_measurement_theta_max      26.4550
_cell_measurement_theta_min      4.1130
_cell_volume                     2420.37(19)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.18(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_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    -83.00 -10.00   1.00    4.00    --  -13.80 -38.00 -30.00   73
  2  \w    -20.00  24.00   1.00    4.00    --  -13.80 -99.00-150.00   44
  3  \w     37.00  76.00   1.00    4.00    --   14.74 178.00  30.00   39
  4  \w    -21.00  28.00   1.00    4.00    --   14.74 -38.00  30.00   49
;
_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      -0.0023620000
_diffrn_orient_matrix_UB_12      -0.0374402000
_diffrn_orient_matrix_UB_13      -0.0117243000
_diffrn_orient_matrix_UB_21      -0.0182131000
_diffrn_orient_matrix_UB_22      0.0109439000
_diffrn_orient_matrix_UB_23      -0.0398050000
_diffrn_orient_matrix_UB_31      0.0889511000
_diffrn_orient_matrix_UB_32      0.0012898000
_diffrn_orient_matrix_UB_33      -0.0046699000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.9977
_diffrn_reflns_Laue_measured_fraction_max 0.9977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9756
_diffrn_reflns_point_group_measured_fraction_full 0.9977
_diffrn_reflns_point_group_measured_fraction_max 0.9977
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88257
_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    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1134.052
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.5913
_refine_diff_density_min         -0.7368
_refine_diff_density_rms         0.1388
_refine_ls_d_res_high            0.8303
_refine_ls_d_res_low             6.0223
_refine_ls_goodness_of_fit_ref   1.0417
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    43
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0417
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.8757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                3232
_reflns_number_total             4422
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2020-0135_suppl.cif
_cod_data_source_block           M-236
_cod_database_code               8105367
_chemical_oxdiff_formula         C1H1O1N1Co1
_reflns_odcompleteness_completeness 99.70
_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 C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O6(H6a,H6b), O7(H7a,H7b)
2.b Free rotating group:
 O8(H8a,H8b)
2.c Ternary CH refined with riding coordinates:
 C9(H9)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18),
 C20(H20), C21(H21), C22(H22), C23(H23)
2.e Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c)
;
_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 1.359
_oxdiff_exptl_absorpt_empirical_full_min 0.787