Synthesis, structures, magnetic and electric properties of four new coordination polymers constructed with heterocyclic nitrogen ligands and multidentate organic acid
Yang, Ru-Xia; Lan, Hai-Ming; Zhu, Peng-Yin; Yang, Li-Zhen; Yu, Yu-Ming; Wang, Lu-Lu; Wang, Duo-Zhi; Inorganica Chimica Acta 506 (2020) 119410–; doi:10.1016/j.ica.2019.119410

data_1564963
_publ_section_title
;
 Synthesis, structures, magnetic and electric properties of four new
 coordination polymers constructed with heterocyclic nitrogen ligands and
 multidentate organic acid
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119410
_journal_paper_doi               10.1016/j.ica.2019.119410
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         'C16 H12 Co N6 O5 S'
_chemical_formula_sum            'C16 H12 Co N6 O5 S'
_chemical_formula_weight         459.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 111.514(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2173(6)
_cell_length_b                   16.6676(8)
_cell_length_c                   11.2467(6)
_cell_measurement_reflns_used    6283
_cell_measurement_temperature    289.0(8)
_cell_measurement_theta_max      28.9500
_cell_measurement_theta_min      3.5820
_cell_volume                     1781.85(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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      289.0(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.885
_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    -60.00  40.00   1.00    3.99    --   11.74 -57.00   0.00  100
  2  \w    -11.00  31.00   1.00    3.99    --   11.74 -99.00 120.00   42
  3  \w    -11.00  78.00   1.00    3.99    --   11.74  57.00 150.00   89
  4  \w    -77.00  21.00   1.00    3.99    --  -11.51 -77.00-120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0416949000
_diffrn_orient_matrix_UB_12      0.0353674000
_diffrn_orient_matrix_UB_13      -0.0139034000
_diffrn_orient_matrix_UB_21      0.0293645000
_diffrn_orient_matrix_UB_22      0.0113406000
_diffrn_orient_matrix_UB_23      -0.0456625000
_diffrn_orient_matrix_UB_31      -0.0543739000
_diffrn_orient_matrix_UB_32      -0.0208655000
_diffrn_orient_matrix_UB_33      -0.0481598000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15466
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.521
_diffrn_reflns_theta_min         3.383
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.293
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4412
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0420P)^2^+2.2658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3723
_reflns_number_total             4412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           exp_657
_cod_original_cell_volume        1781.85(18)
_cod_database_code               1564963
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.867
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 N1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim C2: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
N2 \\sim C3: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Rotating group:
 O5(H5A)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C1(H1), C5(H5), C8(H8), C9(H9), C6(H6), C3(H3),
 C2(H2)
;
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.811