Crystal structure of the 2D coordination polymer poly[diaqua-bis(μ2-3- methoxyisonicotinato-κ2 N:O)cobalt(II)] — dimethylformamide (1/1), C20H30CoN4O10
Sun, Xiao-Tian; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 639–641; doi:10.1515/ncrs-2021-0010

data_8104788
_publ_section_title
;
 Crystal structure of the 2D coordination polymer poly[diaqua-bis(\m2-3-
 methoxyisonicotinato-\k2 N:O)cobalt(II)]&#x00A0;--- dimethylformamide
 (1/1), C20H30CoN4O10
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              639
_journal_page_last               641
_journal_paper_doi               10.1515/ncrs-2021-0010
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C7 H8 Co0.5 N O4, C3 H7 N O'
_chemical_formula_sum            'C10 H15 Co0.5 N2 O5'
_chemical_formula_weight         272.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 113.429(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4752(4)
_cell_length_b                   12.8563(3)
_cell_length_c                   15.0144(5)
_cell_measurement_reflns_used    8087
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0570
_cell_measurement_theta_min      4.2170
_cell_volume                     2386.66(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      293(2)
_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 0.892
_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  25.00   1.00    7.50    --  -13.64 -99.00 -30.00   45
  2  \w    -86.00 -35.00   1.00    7.50    --  -13.64-178.00-180.00   51
  3  \w    -86.00 -34.00   1.00    7.50    --  -13.64 178.00 -90.00   52
  4  \w    -20.00  25.00   1.00    7.50    --  -13.64 -99.00-120.00   45
  5  \w    -20.00  25.00   1.00    7.50    --  -13.64 -99.00  30.00   45
  6  \w    -54.00  34.00   1.00    7.50    --   15.05 -38.00  60.00   88
  7  \w     -4.00  84.00   1.00    7.50    --   15.05  38.00-120.00   88
  8  \w    -56.00  44.00   1.00    7.50    --   15.05 -19.00  60.00  100
  9  \w    -54.00 -22.00   1.00    7.50    --   15.05 -38.00-180.00   32
;
_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      0.0514904000
_diffrn_orient_matrix_UB_12      0.0237400000
_diffrn_orient_matrix_UB_13      0.0138719000
_diffrn_orient_matrix_UB_21      0.0230825000
_diffrn_orient_matrix_UB_22      -0.0393272000
_diffrn_orient_matrix_UB_23      0.0353887000
_diffrn_orient_matrix_UB_31      0.0102814000
_diffrn_orient_matrix_UB_32      -0.0305347000
_diffrn_orient_matrix_UB_33      -0.0347503000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13809
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.469
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0288P)^2^+2.4480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2486
_reflns_number_total             2692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0010_suppl.cif
_cod_data_source_block           xly-55
_cod_original_formula_sum        'C10 H15 Co0.50 N2 O5'
_cod_database_code               8104788
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.772
_reflns_odcompleteness_completeness 99.65
_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:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;